Patent classifications
C07C315/02
Method of synthesising sulforaphane
The present invention relates to a method of synthesising sulforaphane by reacting a compound of formula (A) with an oxidizing agent in an aqueous solvent and in the presence of a catalyst. The invention further provides a method of synthesising a stabilised complex of sulforaphane and cyclodextrin by mixing the sulforaphane prepared by the methodology defined herein with cyclodextrin in an aqueous solvent.
METHOD OF PREPARING A THIOMETHYLPHENOL DERIVATIVE
A method of preparing a thiomethylphenol derivative is disclosed, the method including: (a) carrying out a primary reaction of a phenol derivative represented by the following Chemical Formula 2, a mercaptan derivative represented by R.sub.4SH, and paraformaldehyde at a reaction temperature T.sub.1 under conditions in which a heterocyclic base having 3 to 10 carbon atoms and an acid are simultaneously present; and (b) carrying out a secondary reaction at a reaction temperature T.sub.2 to prepare a thiomethylphenol derivative represented by the following Chemical Formula 1, wherein T.sub.1<T.sub.2 is satisfied.
METHOD OF PREPARING A THIOMETHYLPHENOL DERIVATIVE
A method of preparing a thiomethylphenol derivative is disclosed, the method including: (a) carrying out a primary reaction of a phenol derivative represented by the following Chemical Formula 2, a mercaptan derivative represented by R.sub.4SH, and paraformaldehyde at a reaction temperature T.sub.1 under conditions in which a heterocyclic base having 3 to 10 carbon atoms and an acid are simultaneously present; and (b) carrying out a secondary reaction at a reaction temperature T.sub.2 to prepare a thiomethylphenol derivative represented by the following Chemical Formula 1, wherein T.sub.1<T.sub.2 is satisfied.
CONTINUOUS-FLOW PREPARATION METHOD OF DIOL SULFONE
A continuous-flow preparation method of diol sulfone using a two-stage micro-reaction system. The system includes a first micro-mixer, a first micro-channel reactor, a second micro-mixer, and a second micro-channel reactor communicated in sequence. The method includes: feeding hydrogen peroxide, a catalyst and a diol thioether solution simultaneously to the first micro-mixer followed by mixing; feeding the reaction mixture to the first micro-channel reactor for continuous oxidation; and feeding the reaction mixture and water simultaneously to the second micro-mixer and the second micro-channel reactor for continuous quenching and crystallization to obtain diol sulfone.
CONTINUOUS-FLOW PREPARATION METHOD OF DIOL SULFONE
A continuous-flow preparation method of diol sulfone using a two-stage micro-reaction system. The system includes a first micro-mixer, a first micro-channel reactor, a second micro-mixer, and a second micro-channel reactor communicated in sequence. The method includes: feeding hydrogen peroxide, a catalyst and a diol thioether solution simultaneously to the first micro-mixer followed by mixing; feeding the reaction mixture to the first micro-channel reactor for continuous oxidation; and feeding the reaction mixture and water simultaneously to the second micro-mixer and the second micro-channel reactor for continuous quenching and crystallization to obtain diol sulfone.
PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone comprising reacting a solution comprising 4,4′-dichlorodiphenyl sulfoxide and at least one linear C.sub.6-C.sub.10 carboxylic acid as solvent with an oxidizing agent to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone, wherein the concentration of water in the reaction mixture is kept below 5 wt %, the process comprising: (a) adding 0.9 to 1.05 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide uniformly distributed to the solution at a temperature in the range from 80 to 105° C. over a period from 1.5 to 5 h in a first step to obtain the reaction mixture; (b) agitating the reaction mixture after completion of the first step at the temperature of the first step for 5 to 30 min without adding oxidizing agent; (c) adding 0.05 to 0.2 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide to the reaction mixture at a temperature in the range from 80 to 105° C. over a period of less than 40 min in a second step; (d) agitating the reaction mixture after completion of the second step at the temperature of the second step for 10 to 30 min without adding oxidizing agent, (e) heating the reaction mixture to a temperature in the range from 95 to 110° C. and hold this temperature for 10 to 90 min to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone.
PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone comprising reacting a solution comprising 4,4′-dichlorodiphenyl sulfoxide and at least one linear C.sub.6-C.sub.10 carboxylic acid as solvent with an oxidizing agent to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone, wherein the concentration of water in the reaction mixture is kept below 5 wt %, the process comprising: (a) adding 0.9 to 1.05 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide uniformly distributed to the solution at a temperature in the range from 80 to 105° C. over a period from 1.5 to 5 h in a first step to obtain the reaction mixture; (b) agitating the reaction mixture after completion of the first step at the temperature of the first step for 5 to 30 min without adding oxidizing agent; (c) adding 0.05 to 0.2 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide to the reaction mixture at a temperature in the range from 80 to 105° C. over a period of less than 40 min in a second step; (d) agitating the reaction mixture after completion of the second step at the temperature of the second step for 10 to 30 min without adding oxidizing agent, (e) heating the reaction mixture to a temperature in the range from 95 to 110° C. and hold this temperature for 10 to 90 min to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone.
PROCESS FOR PRODUCING 4,4'-DICHLORODIPHENYL SULFONE
The invention relates to a process for producing 4,4′-dichlorodiphenyl sulfone comprising reacting a solution comprising 4,4′-dichlorodiphenyl sulfoxide and at least one linear C.sub.6-C.sub.10 carboxylic acid as solvent with an oxidizing agent to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone, wherein the concentration of water in the reaction mixture is kept below 5 wt %, the process comprising: (a) adding 0.9 to 1.05 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide uniformly distributed to the solution at a temperature in the range from 80 to 105° C. over a period from 1.5 to 5 h in a first step to obtain the reaction mixture; (b) agitating the reaction mixture after completion of the first step at the temperature of the first step for 5 to 30 min without adding oxidizing agent; (c) adding 0.05 to 0.2 mol oxidizing agent per mol 4,4′-dichlorodiphenyl sulfoxide to the reaction mixture at a temperature in the range from 80 to 105° C. over a period of less than 40 min in a second step; (d) agitating the reaction mixture after completion of the second step at the temperature of the second step for 10 to 30 min without adding oxidizing agent, (e) heating the reaction mixture to a temperature in the range from 95 to 110° C. and hold this temperature for 10 to 90 min to obtain a crude reaction product comprising 4,4′-dichlorodiphenyl sulfone.
CHEMOENZYMATIC PROCESS FOR COPRODUCTION OF A DISULFIDE AND A SULFOXIDE OR A SULFONE
Chemoenzymatic process for coproducing a disulfide and a sulfoxide or a sulfone The present invention relates to a chemoenzymatic process for coproducing disulfide and sulfoxide or sulfone from a composition M comprising: 1) a sulfide, 2) optionally an oxidizing agent, 3) an organic compound bearing at least one thiol group, 4) an enzyme E catalyzing the oxidation of said sulfide to sulfoxide or to sulfone, 5) an enzyme D catalyzing the formation of a disulfide bridge between two equivalents of said organic compound bearing at least one thiol group to form a dimer, and 6) a cofactor common to the two enzymes E and D; and also to a composition enabling especially the implementation of this process. The present invention also relates to the use of a mercaptan for reducing a disulfide bridge formed between two equivalents of an organic compound bearing at least one thiol group, and more particularly to the use thereof as regeneration substrate of the process described above.
CHEMOENZYMATIC PROCESS FOR COPRODUCTION OF A DISULFIDE AND A SULFOXIDE OR A SULFONE
Chemoenzymatic process for coproducing a disulfide and a sulfoxide or a sulfone The present invention relates to a chemoenzymatic process for coproducing disulfide and sulfoxide or sulfone from a composition M comprising: 1) a sulfide, 2) optionally an oxidizing agent, 3) an organic compound bearing at least one thiol group, 4) an enzyme E catalyzing the oxidation of said sulfide to sulfoxide or to sulfone, 5) an enzyme D catalyzing the formation of a disulfide bridge between two equivalents of said organic compound bearing at least one thiol group to form a dimer, and 6) a cofactor common to the two enzymes E and D; and also to a composition enabling especially the implementation of this process. The present invention also relates to the use of a mercaptan for reducing a disulfide bridge formed between two equivalents of an organic compound bearing at least one thiol group, and more particularly to the use thereof as regeneration substrate of the process described above.