C07C315/02

POROUS LAYERED TRANSITION METAL DICHALCOGENIDE AND PREPARATION METHOD AND USE THEREOF

The present invention relates to the field of catalysts, and provides a porous layered transition metal dichalcogenide (TMD) and a preparation method and use thereof. The preparation method includes the following steps: (1) mixing silica microspheres, a transition metal salt and an elemental chalcogen, and pressing to obtain a tablet, the silica microspheres having a same or different particle diameters; and (2) sintering the tablet under hydrogen, and removing the silica microspheres to obtain the porous layered TMD. The porous layered TMD prepared by the method of the present invention has a high lattice edge exposure, which provides more active sites and higher catalytic activity, so the porous layered TMD can effectively catalyze the oxidation of alcohols to aldehydes or sulfides to sulfoxides under visible light irradiation.

POROUS LAYERED TRANSITION METAL DICHALCOGENIDE AND PREPARATION METHOD AND USE THEREOF

The present invention relates to the field of catalysts, and provides a porous layered transition metal dichalcogenide (TMD) and a preparation method and use thereof. The preparation method includes the following steps: (1) mixing silica microspheres, a transition metal salt and an elemental chalcogen, and pressing to obtain a tablet, the silica microspheres having a same or different particle diameters; and (2) sintering the tablet under hydrogen, and removing the silica microspheres to obtain the porous layered TMD. The porous layered TMD prepared by the method of the present invention has a high lattice edge exposure, which provides more active sites and higher catalytic activity, so the porous layered TMD can effectively catalyze the oxidation of alcohols to aldehydes or sulfides to sulfoxides under visible light irradiation.

Processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac

The disclosure provides processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac, relating to the field of medicine. The former comprises mixing 6-fluoro-2-methyl-1-indanone, cyanoacetic acid, a first organic solvent and an acetic acid-based catalyst to proceed with a first condensation reaction to give a first condensation reaction solution, which contains 5-fluoro-2-methyl-3-indanacetonitrile; and mixing the first condensation reaction solution, per se, with a base, a second organic solvent and 4-(methylthio)benzaldehyde to proceed with a second condensation reaction to give 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile. The process is a one-pot process without separation of 5-fluoro-2-methyl-3-indanacetonitrile from the solvent, shortening the synthetic route, simplifying the preparation process and improving the 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile yield.

Processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac

The disclosure provides processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac, relating to the field of medicine. The former comprises mixing 6-fluoro-2-methyl-1-indanone, cyanoacetic acid, a first organic solvent and an acetic acid-based catalyst to proceed with a first condensation reaction to give a first condensation reaction solution, which contains 5-fluoro-2-methyl-3-indanacetonitrile; and mixing the first condensation reaction solution, per se, with a base, a second organic solvent and 4-(methylthio)benzaldehyde to proceed with a second condensation reaction to give 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile. The process is a one-pot process without separation of 5-fluoro-2-methyl-3-indanacetonitrile from the solvent, shortening the synthetic route, simplifying the preparation process and improving the 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile yield.

Processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac

The disclosure provides processes for preparing 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile and for preparing sulindac, relating to the field of medicine. The former comprises mixing 6-fluoro-2-methyl-1-indanone, cyanoacetic acid, a first organic solvent and an acetic acid-based catalyst to proceed with a first condensation reaction to give a first condensation reaction solution, which contains 5-fluoro-2-methyl-3-indanacetonitrile; and mixing the first condensation reaction solution, per se, with a base, a second organic solvent and 4-(methylthio)benzaldehyde to proceed with a second condensation reaction to give 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile. The process is a one-pot process without separation of 5-fluoro-2-methyl-3-indanacetonitrile from the solvent, shortening the synthetic route, simplifying the preparation process and improving the 5-fluoro-2-methyl-1-(4-methylthiobenzylidene)-3-indanacetonitrile yield.

PROCESS FOR SYNTHESIZING TRIARYLMETHANE SULFONE COMPOUNDS

A process for synthesizing a compound of formula (I)

##STR00001##

including: (a) condensing the benzaldehyde compound of formula (II) with the dialkylaniline of formula (III) to give the triphenylmethane of formula (IV); (b) treating the triphenylmethane of formula (IV) with sulfuric acid to form the triphenylmethane sulfone of the formula (V); and (c) oxidizing the triphenylmethane sulfone of formula (V) with a quinone. Such a process may be used to prepare patent blue.

PROCESS FOR SYNTHESIZING TRIARYLMETHANE SULFONE COMPOUNDS

A process for synthesizing a compound of formula (I)

##STR00001##

including: (a) condensing the benzaldehyde compound of formula (II) with the dialkylaniline of formula (III) to give the triphenylmethane of formula (IV); (b) treating the triphenylmethane of formula (IV) with sulfuric acid to form the triphenylmethane sulfone of the formula (V); and (c) oxidizing the triphenylmethane sulfone of formula (V) with a quinone. Such a process may be used to prepare patent blue.

A PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising carboxylic acid; (c) purifying the second stream comprising carboxylic acid by distilling a part of the second stream comprising carboxylic acid stripping low boilers from at least a part of the second stream comprising carboxylic acid (d) recycling the purified carboxylic acid into the reaction (a).

A PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising carboxylic acid; (c) purifying the second stream comprising carboxylic acid by distilling a part of the second stream comprising carboxylic acid stripping low boilers from at least a part of the second stream comprising carboxylic acid (d) recycling the purified carboxylic acid into the reaction (a).

A PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE

The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone, comprising: (a) reacting 4,4′-dichlorodiphenyl sulfoxide and an oxidizing agent in at least one carboxylic acid as solvent to obtain a reaction mixture comprising 4,4′-dichlorodiphenyl sulfone and carboxylic acid; (b) separating the reaction mixture into a first stream comprising 4,4′-dichlorodiphenyl sulfone and a second stream comprising carboxylic acid; (c) purifying the second stream comprising carboxylic acid by distilling a part of the second stream comprising carboxylic acid stripping low boilers from at least a part of the second stream comprising carboxylic acid (d) recycling the purified carboxylic acid into the reaction (a).