GOLD (I) GEFITINIB DERIVATIVES AND PREPARATION METHOD AND APPLICATION THEREOF
20250154179 ยท 2025-05-15
Assignee
- TONGJI HOSPITAL, TONGJI MEDICAL COLLEGE, HUAZHONG UNIVERSITY OF SCIENCE AND TECHNOLOGY (Wuhan City, CN)
- SHANXI BETHUNE HOSPITAL (SHANXI ACADEMY OF MEDICAL SCIENCES) (Taiyuan City, CN)
- NANJING UNIVERSITY OF CHINESE MEDICINE (Nanjing City, CN)
Inventors
- Shuang Wei (Wuhan City, CN)
- Wukun Liu (Wuhan City, CN)
- Lingling Wang (Wuhan City, CN)
- Xiaoyan Ma (Wuhan City, CN)
- Jia Wei (Wuhan City, CN)
- Xiansheng Liu (Wuhan City, CN)
- Xueli Bai (Wuhan City, CN)
- Huiguo Liu (Wuhan City, CN)
Cpc classification
A61K31/675
HUMAN NECESSITIES
International classification
Abstract
The invention discloses a class of gold (I) Gefitinib derivatives, their preparation methods, and applications. The methods for preparing the gold (I) Gefitinib derivatives comprise the following steps: 1) Dissolve compound I and potassium hydroxide in methanol, and add a gold ligand II to obtain a mixture; 2) Stir the mixture for reaction, and then filter under reduced pressure to obtain a crude product; 3) Purify the crude product to obtain the gold (I) Gefitinib derivatives. One of the gold (I) Gefitinib derivatives has an EGFR/TrxR dual-target anti-lung cancer effect, retaining the stem nucleus structure of Gefitinib, 4-aniline-quinazoline, to ensure its original EGFR targeting inhibition activity, and introducing alkynyl groups with different carbon chain lengths to connect different gold ligands so that it can target both EGFR and TrxR simultaneously, enhancing its anti-lung cancer activity and overcoming the resistance of lung cancer to Gefitinib.
Claims
1-10. (canceled)
11. A gold (I) Gefitinib derivative, wherein the gold (I) Gefitinib derivative has a structural formula as follows: ##STR00025## where n is selected from 1, 2, 3, 4 and 5; R.sub.1 is selected from methoxy, acetyl, hydroxyl, 4-propyl morpholine and 2-methoxyethoxy; R.sub.2 and R.sub.3 are selected from hydrogen, halogen and CN; R.sub.4 is selected from hydrogen, alkyl and 4-propyl morpholine; and R.sub.5 is selected from triphenylphosphine, triethylphosphine, tricyclohexylphosphine, 1,3,5-triaza-7-phosphaadamantane, 1,3-diethylimidazole, 1,3-diethyl-4,5-bis(4-methoxyphenyl)imidazole, 1,3-diethyl-4,5-bis(4-fluorophenyl)imidazole, 1-(anthracene-9-methyl)-3-ethyl-4,5-bis(4-fluorophenyl)imidazole, 1-(anthracene-9-methyl)-3-ethyl-4,5-bis(4-methoxy phenyl)imidazole, 1,3-diethyl-4,5-bis(biphenyl)imidazole and 1,3-diethyl-4,5-bis(4-fluoro-[1,1-biphenyl])imidazole.
12. A method for preparing the gold (I) Gefitinib derivative according to claim 11, wherein the method comprises the following steps: 1) dissolving a compound I and potassium hydroxide in methanol and adding a gold ligand II to obtain a mixture; 2) stirring the mixture for reaction and then filtering under reduced pressure to obtain a crude product; 3) purifying the crude product to obtain the gold (I) Gefitinib derivatives; wherein the structural formula of the compound I is as follows: ##STR00026## where n is selected from 1, 2, 3, 4 and 5; R.sub.1 is selected from methoxy, acetyl, hydroxyl, 4-propyl morpholine and 2-methoxyethoxy; R.sub.2 and R.sub.3 are selected from hydrogen, halogen and CN; R.sub.4 is selected from hydrogen, alkyl and 4-propyl morpholine; wherein the structural formula of the gold ligand II is as follows:
R.sub.5AuX where R.sub.5 is selected from triphenylphosphine, triethylphosphine, tricyclohexylphosphine, 1,3,5-triaza-7-phosphaadamantane, 1,3-diethylimidazole, 1,3-diethyl-4,5-bis(4-methoxyphenyl)imidazole, 1,3-diethyl-4,5-bis(4-fluorophenyl)imidazole, 1-(anthracene-9-methyl)-3-ethyl-4,5-bis(4-fluorophenyl)imidazole, 1-(anthracene-9-methyl)-3-ethyl-4,5-bis(4-methoxy phenyl)imidazole, 1,3-diethyl-4,5-bis(biphenyl)imidazole and 1,3-diethyl-4,5-bis(4-fluoro-[1,1-biphenyl])imidazole; and X is selected from chlorine and bromine.
13. The preparation method according to claim 12, wherein in step 1), the solid-liquid ratio of the compound I to methanol is (0.010.1) mmol:1 ml.
14. The preparation method according to claim 13, wherein in step 1), the solid-liquid ratio of the compound I to methanol is 0.0923 mmol:1 ml.
15. The preparation method according to claim 12, wherein in step 1), the molar ratio of potassium hydroxide to the gold ligand II is (0.21):(0.020.1).
16. The preparation method according to claim 12, wherein in step 1), the molar ratio of the compound I to the gold ligand II is (0.050.1):(0.030.1).
17. The preparation method according to claim 12, wherein in step 2), the mixture is stirred for reaction at 2535 C.
18. The preparation method according to claim 17, wherein in step 2), the mixture is stirred for reaction for 0.510 h.
19. The preparation method according to claim 12, wherein in step 3), the crude product is purified by means of methanol washing or silica gel column chromatography.
20. An application of the gold (I) Gefitinib derivative according to claim 11, wherein the gold (I) Gefitinib derivative is used to prepare a drug treating lung cancer resistant to EGFR-TKI.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0040]
[0041]
[0042]
[0043]
DETAILED DESCRIPTION
[0044] Below the implementation of the present invention is elaborated in conjunction with embodiments. The embodiments are not intended to limit the present invention and are examples only. Through the elaboration, the advantages of the present invention will become more apparent and understandable.
Embodiment 1
[0045] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00003##
[0046] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0047] 1) dissolving a compound I (0.139 mmol) in methanol (15 ml), then adding potassium hydroxide (0.749 mmol), stirring them at room temperature for 5 min and then adding chloro (triphenylphosphine) gold (I) (0.110 mmol) to obtain a mixture; [0048] wherein the structural formula of the compound I is as follows:
##STR00004## [0049] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0050] 2) stirring the mixture for reaction at 25 C. for 6 h and then filtering under reduced pressure to obtain a crude product; [0051] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a white solid, with a yield of 56.58%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.56 (s, 1H), 8.51 (s, 1H), 8.14-8.09 (m, 1H), 7.87 (s, 1H), 7.79 (dt, J=7.7, 3.3 Hz, 1H), 7.67-7.39 (m, 16 h), 7.22 (s, 1H), 4.97 (s, 2H), 3.95 (s, 3H). 13C NMR (126 MHz, DMSO-d.sub.6) 156.53, 155.12, 153.22, 147.66, 147.57, 134.38, 134.27, 132.44, 130.13, 130.04, 129.80, 123.91, 122.77, 122.71, 117.10, 116.93, 107.80, 103.72, 58.24, 56.33. ESI-MS m/z [M].sup.+ calc.: 816.02 found: 816.63.
Embodiment 2
[0052] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00005##
[0053] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0054] 1) dissolving a compound I (0.057 mmol) in methanol (10 ml), then adding potassium hydroxide (0.210 mmol), stirring them at room temperature for 5 min and then adding (1,3,5-triaza-7-phosphaadamantane)-gold chloride (0.033 mmol) to obtain a mixture; [0055] wherein the structural formula of the compound I is as follows:
##STR00006## [0056] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0057] 2) stirring the mixture for reaction at 25 C. for 1.5 h and then filtering under reduced pressure to obtain a crude product; [0058] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a light-yellow solid, with a yield of 66.11%. 1H NMR (500 MHZ, DMSO-d.sub.6) 9.52 (d, J=2.2 Hz, 1H), 8.51 (s, 1H), 8.12 (ddd, J=7.2, 4.6, 2.6 Hz, 1H), 7.84-7.76 (m, 2H), 7.50-7.43 (m, 1H), 7.21 (s, 1H), 4.90 (s, 2H), 4.46 (d, J=12.8 Hz, 3H), 4.32 (d, J=13.0 Hz, 3H), 4.22 (s, 6 h), 3.94 (d, J=1.9 Hz, 3H). 13C NMR (126 MHZ, DMSO-d.sub.6) 156.48, 155.15, 153.18, 152.63, 147.57, 147.53, 137.27, 123.78, 122.66, 122.60, 119.21, 117.14, 116.97, 109.09, 107.76, 103.78, 72.30, 72.24, 58.21, 56.32, 56.24, 51.21, 51.05. ESI-MS m/z [M+H].sup.+ calc.: 711.88 found: 711.70.
Embodiment 3
[0059] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00007##
[0060] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0061] 1) dissolving a compound I (0.056 mmol) in methanol (10 ml), then adding potassium hydroxide (0.203 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethylimidazole gold bromide (0.028 mmol) to obtain a mixture; [0062] wherein the structural formula of the compound I is as follows:
##STR00008## [0063] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0064] 2) stirring the mixture for reaction at 25 C. for 4 h and then evaporating the solvent to obtain a crude product; [0065] 3) subjecting the crude product to silica gel column chromatography (the eluent is EA:PE=1:10 till EA gradient elution) to obtain the gold (I) Gefitinib derivatives, which form a yellow solid, with a yield of 27.98%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.56 (s, 1H), 8.51 (s, 1H), 8.12 (dd, J=6.9, 2.7 Hz, 1H), 7.87-7.78 (m, 2H), 7.45 (d, J=7.8 Hz, 3H), 7.22 (s, 1H), 4.93 (s, 2H), 4.09 (q, J=7.2 Hz, 4H), 3.96 (s, 3H), 1.34 (t, J=7.3 Hz, 6 h). 13C NMR (126 MHZ, DMSO-d.sub.6) 184.17, 156.51, 155.14, 153.14, 152.63, 147.82, 147.50, 123.87, 122.75, 122.16, 121.47, 117.10, 116.93, 109.15, 107.74, 103.58, 97.59, 58.66, 56.30, 46.10, 45.80, 29.50, 17.33, 17.13. ESI-MS m/z [M+H].sup.+ calc.: 678.91 found: 678.53.
Embodiment 4
[0066] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00009##
[0067] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0068] 1) dissolving a compound I (0.064 mmol) in methanol (10 ml), then adding potassium hydroxide (0.237 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethyl-4,5-bis(4-methoxyphenyl)imidazole gold bromide (0.033 mmol) to obtain a mixture; [0069] wherein the structural formula of the compound I is as follows:
##STR00010## [0070] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0071] 2) stirring the mixture for reaction at 25 C. for 1 h and then filtering under reduced pressure to obtain a crude product; [0072] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a white solid, with a yield of 84.95%, 1H NMR (500 MHz, DMSO-d.sub.6) 9.56 (s, 1H), 8.51 (s, 1H), 8.12 (dd, J=6.8, 2.7 Hz, 1H), 7.87 (s, 1H), 7.81 (ddd, J=9.1, 4.3, 2.7 Hz, 1H), 7.45 (t, J=9.1 Hz, 1H), 7.29-7.24 (m, 4H), 7.22 (s, 1H), 6.97-6.91 (m, 4H), 4.96 (s, 2H), 4.02 (q, J=7.2 Hz, 4H), 3.96 (s, 3H), 3.75 (s, 6 h), 1.17 (t, J=7.2 Hz, 6 h). 13C NMR (126 MHZ, DMSO-d.sub.6) 183.79, 160.11, 156.49, 155.13, 153.14, 147.84, 147.51, 132.50, 131.01, 123.85, 122.72, 122.67, 120.07, 117.10, 116.92, 114.61, 109.15, 107.75, 103.57, 97.76, 58.71, 56.31, 55.59, 43.90, 17.19. ESI-MS m/z [M].sup.+ calc.: 890.16 found: 890.87.
Embodiment 5
[0073] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00011##
[0074] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0075] 1) dissolving a compound I (0.056 mmol) in methanol (10 ml), then adding potassium hydroxide (0.203 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethyl-4,5-bis(4-fluorophenyl)imidazole gold bromide (0.028 mmol) to obtain a mixture; [0076] wherein the structural formula of the compound I is as follows:
##STR00012## [0077] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0078] 2) stirring the mixture for reaction at 25 C. for 5 h and then evaporating the solvent to obtain a crude product [0079] 3) subjecting the crude product to silica gel column chromatography (the eluent is EA:PE=1:20 till EA:PE=1:1 gradient elution) to obtain the gold (I) Gefitinib derivatives, which form a while solid, with a yield of 39.68%. 1H NMR (500 MHZ, Chloroform-d) 8.51 (s, 1H), 8.47 (s, 1H), 8.42 (s, 1H), 7.67 (dd, J=6.7, 2.7 Hz, 1H), 7.48 (ddd, J=9.0, 4.2, 2.7 Hz, 1H), 6.98 (d, J=7.2 Hz, 8H), 6.89-6.80 (m, 2H), 5.73 (s, 2H), 3.90 (s, 3H), 3.59 (q, J=7.2 Hz, 4H), 0.80 (t, J=7.2 Hz, 6 h). 13C NMR (126 MHZ, Chloroform-d) 184.14, 164.05, 162.05, 155.40, 154.48, 152.77, 147.22, 132.24, 132.17, 130.28, 128.41, 123.29, 123.27, 122.13, 120.08, 116.23, 116.06, 115.22, 108.98, 106.93, 103.13, 103.01, 58.01, 55.92, 43.67, 16.63. ESI-MS m/z [M].sup.+ calc.: 866.09 found: 866.65.
Embodiment 6
[0080] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00013##
[0081] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0082] 1) dissolving a compound I (0.056 mmol) in methanol (10 ml), then adding potassium hydroxide (0.203 mmol), stirring them at room temperature for 5 min and then adding 1-(anthracene-9-methyl)-3-ethyl-4,5-bis(4-methoxy phenyl) imidazole gold chloride (0.028 mmol) to obtain a mixture; [0083] wherein the structural formula of the compound I is as follows:
##STR00014## [0084] where n=1, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0085] 2) stirring the mixture for reaction at 25 C. for 4.5 h and then filtering under reduced pressure to obtain a crude product; [0086] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a yellow solid, with a yield of 36.73%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.52 (s, 1H), 8.46 (s, 1H), 8.42 (s, 1H), 8.19-8.14 (m, 2H), 8.05 (dd, J=6.8, 2.7 Hz, 1H), 7.95-7.90 (m, 2H), 7.85 (s, 1H), 7.75 (ddd, J=9.1, 4.3, 2.7 Hz, 1H), 7.41-7.33 (m, 5H), 7.21-7.15 (m, 3H), 7.10 (t, J=8.8 Hz, 2H), 6.53-6.47 (m, 2H), 6.44-6.37 (m, 4H), 4.95 (s, 2H), 4.07 (q, J=7.2 Hz, 2H), 3.92 (s, 3H), 1.15 (t, J=7.2 Hz, 3H). 13C NMR (126 MHz, DMSO-d.sub.6) 186.08, 161.77, 161.01, 156.46, 155.12, 154.50, 153.04, 147.75, 147.36, 137.15, 133.25, 133.18, 132.69, 132.63, 131.44, 131.11, 130.88, 130.59, 129.37, 129.31, 126.80, 125.91, 125.20, 124.06, 123.86, 123.71, 123.48, 122.59, 122.54, 119.29, 119.15, 116.98, 116.81, 116.30, 116.13, 114.99, 114.82, 109.13, 107.55, 103.53, 97.72, 58.51, 56.26, 47.73, 44.33, 31.72, 31.59, 29.43, 29.13, 22.53, 17.14, 14.39. ESI-MS m/z [M].sup.+ calc.: 1028.28 found: 1028.71.
Embodiment 7
[0087] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00015##
[0088] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0089] 1) dissolving a compound I (0.052 mmol) in methanol (5 ml), then adding potassium hydroxide (0.203 mmol), stirring them at room temperature for 5 min and then adding triphenylphosphine gold chloride (0.028 mmol) to obtain a mixture; [0090] wherein the structural formula of the compound I is as follows:
##STR00016## [0091] where n=3, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H. [0092] 2) stirring the mixture for reaction at 25 C. for 4.5 h and then filtering under reduced pressure to obtain a crude product; [0093] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a while solid, with a yield of 69.47%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.58 (s, 1H), 8.50 (s, 1H), 8.09 (dd, J=6.9, 2.7 Hz, 1H), 7.84 (s, 1H), 7.78 (ddd, J=9.0, 4.3, 2.6 Hz, 1H), 7.62-7.55 (m, 9H), 7.53-7.41 (m, 7H), 7.22 (s, 1H), 4.26 (t, J=6.1 Hz, 2H), 3.95 (s, 3H), 2.42 (t, J=6.8 Hz, 2H), 1.98 (p, J=6.4 Hz, 2H). 13C NMR (126 MHz, DMSO-d.sub.6) 156.49, 154.94, 153.09, 148.84, 147.44, 134.35, 134.24, 132.33, 132.31, 130.15, 130.07, 129.98, 129.71, 124.03, 122.90, 122.85, 119.29, 117.04, 116.87, 109.27, 107.77, 102.88, 67.99, 56.36, 29.29, 16.71. ESI-MS m/z [M].sup.+ calc.: 844.07 found: 844.73.
Embodiment 8
[0094] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00017##
[0095] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0096] 1) dissolving a compound I (0.063 mmol) in methanol (5 ml), then adding potassium hydroxide (0.310 mmol), stirring them at room temperature for 5 min and then adding (1,3,5-triaza-7-phosphaadamantane)-gold chloride (0.050 mmol) to obtain a mixture; [0097] wherein the structural formula of the compound I is as follows:
##STR00018## [0098] where n=3, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H. [0099] 2) stirring the mixture for reaction at 25 C. for 1 h and then filtering under reduced pressure to obtain a crude product; [0100] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a while solid, with a yield of 86.42%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.59 (s, 1H), 8.50 (s, 1H), 8.12 (dd, J=6.8, 2.6 Hz, 1H), 7.83-7.79 (m, 2H), 7.46 (t, J=9.1 Hz, 1H), 7.21 (s, 1H), 4.47 (d, J=12.7 Hz, 3H), 4.32 (d, J=13.0 Hz, 3H), 4.21 (d, J=7.6 Hz, 8H), 3.94 (s, 3H), 2.33 (t, J=6.8 Hz, 2H), 1.92 (p, J=6.5 Hz, 2H). 13C NMR (126 MHZ, DMSO-d.sub.6) 156.48, 154.94, 153.09, 148.87, 147.44, 137.28, 124.02, 122.89, 122.83, 117.08, 116.91, 109.24, 107.77, 102.80, 72.32, 72.26, 67.96, 56.35, 51.24, 51.08, 29.37, 16.72. ESI-MS m/z [M+H].sup.+ calc.: 739.94 found: 739.81.
Embodiment 9
[0101] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00019##
[0102] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0103] 1) dissolving a compound I (0.052 mmol) in methanol (5 ml), then adding potassium hydroxide (0.260 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethylimidazole gold bromide (0.056 mmol) to obtain a mixture; [0104] wherein the structural formula of the compound I is as follows:
##STR00020## [0105] where n=3, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H. [0106] 2) stirring the mixture for reaction at 25 C. for 9 h and then filtering under reduced pressure to obtain a crude product; [0107] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a yellow solid, with a yield of 15.30%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.60 (s, 1H), 8.50 (s, 1H), 8.11 (dd, J=6.9, 2.7 Hz, 1H), 7.89-7.75 (m, 2H), 7.43 (d, J=16.2 Hz, 3H), 7.21 (s, 1H), 4.26 (t, J=6.0 Hz, 2H), 4.08 (q, J=7.3 Hz, 5H, OCH.sub.3), 3.95 (s, 2H), 2.39 (d, J=6.7 Hz, 2H), 1.95 (t, J=6.5 Hz, 2H), 1.33 (t, J=7.2 Hz, 6 h). 13C NMR (126 MHZ, DMSO-d.sub.6) 185.03, 172.64, 156.48, 154.95, 153.04, 148.91, 147.42, 137.29, 123.99, 122.86, 122.81, 122.15, 121.30, 117.04, 116.87, 107.75, 102.81, 68.12, 60.23, 56.34, 46.10, 45.72, 29.59, 21.63, 17.33, 17.09. ESI-MS m/z [M+H].sup.+ calc.: 706.97 found: 706.58.
Embodiment 10
[0108] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00021##
[0109] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0110] 1) dissolving a compound I (0.028 mmol) in methanol (5 ml), then adding potassium hydroxide (0.135 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethyl-4,5-bis(4-methoxyphenyl)imidazole gold bromide (0.020 mmol) to obtain a mixture; [0111] wherein the structural formula of the compound I is as follows:
##STR00022## [0112] where n=3, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H. [0113] 2) stirring the mixture for reaction at 25 C. for 5 h and then filtering under reduced pressure to obtain a crude product; [0114] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a while solid, with a yield of 83.16%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.59 (s, 1H), 8.50 (s, 1H), 8.12 (dd, J=6.9, 2.7 Hz, 1H), 7.86 (s, 1H), 7.82 (ddt, J=9.1, 4.3, 2.0 Hz, 1H), 7.44 (t, J=9.1 Hz, 1H), 7.30-7.20 (m, 5H), 6.97-6.91 (m, 4H), 4.27 (t, J=6.1 Hz, 2H), 4.02 (q, J=7.2 Hz, 4H), 3.96 (s, 3H), 3.75 (s, 6 h), 2.41 (t, J=6.9 Hz, 2H), 1.97 (p, J=6.6 Hz, 2H), 1.15 (t, J=7.2 Hz, 6 h). 13C NMR (126 MHZ, DMSO-d.sub.6) 184.68, 160.08, 156.48, 154.97, 153.05, 147.42, 137.28, 132.48, 130.85, 123.98, 122.86, 122.80, 121.29, 120.16, 119.14, 117.05, 116.88, 114.60, 109.26, 107.76, 103.04, 102.82, 68.15, 56.36, 55.58, 43.82, 29.55, 17.14, 17.10. ESI-MS m/z [M].sup.+ calc.: 918.22 found: 918.87.
Embodiment 11
[0115] A gold (I) Gefitinib derivative in this embodiment, with a structural formula as follows:
##STR00023##
[0116] A method for preparing the gold (I) Gefitinib derivative in this embodiment, comprising the following steps: [0117] 1) dissolving a compound I (0.041 mmol) in methanol (5 ml), then adding potassium hydroxide (0.232 mmol), stirring them at room temperature for 5 min and then adding 1,3-diethyl-4,5-bis(4-fluorophenyl)imidazole gold bromide (0.031 mmol) to obtain a mixture; [0118] wherein the structural formula of the compound I is as follows:
##STR00024## [0119] where n=3, R.sub.1OCH.sub.3, R.sub.2Cl, R.sub.3F, R.sub.4H; [0120] 2) stirring the mixture for reaction at 25 C. for 4 h and then filtering under reduced pressure to obtain a crude product; [0121] 3) washing the crude product with methanol to obtain the gold (I) Gefitinib derivatives, which form a while solid, with a yield of 54.84%. 1H NMR (500 MHz, DMSO-d.sub.6) 9.59 (s, 1H), 8.50 (s, 1H), 8.12 (dd, J=6.9, 2.6 Hz, 1H), 7.86 (s, 1H), 7.82 (ddd, J=9.0, 4.3, 2.6 Hz, 1H), 7.47-7.38 (m, 5H), 7.29-7.20 (m, 5H), 4.27 (t, J=6.2 Hz, 2H), 4.04 (q, J=7.2 Hz, 4H), 3.96 (s, 3H), 2.41 (t, J=6.8 Hz, 2H), 1.97 (p, J=6.4 Hz, 2H), 1.16 (t, J=7.2 Hz, 6 h). 13C NMR (126 MHz, DMSO-d.sub.6) 185.33, 161.92, 156.48, 154.97, 153.05, 148.91, 147.43, 137.31, 133.54, 133.48, 130.45, 123.97, 122.85, 117.05, 116.88, 116.42, 116.25, 109.26, 107.78, 102.83, 68.15, 56.36, 44.00, 29.56, 17.06. ESI-MS m/z [M].sup.+ calc.: 894.15 found: 894.70.
Effect Example
[0122] The present invention further provides an application of a gold (I) Gefitinib derivative, mainly providing the study of the effect of Embodiment 8 (L1Au2 for short).
[0123] The above are only some embodiments of the present invention. It should be noted that all the variations or replacements within the scope of the technology revealed by the present, which can be readily thought of by any person skilled in the art, shall fall within the scope of protection of the present invention, and the rest not described in detail is prior art.