On June 10, 2015, Chen, Zhengwei; Xiao, Tao; Zhu, Jiahao; Yu, Chuanzong; Dai, Jianxin published a patent.Quality Control of (2-Fluorophenyl)methanethiol The title of the patent was Preparation method of 6-substituted-2-trifluoromethyl benzene sulfonyl chloride. And the patent contained the following:
The present invention refers to the preparation method of 6-substituted-2-trifluoromethyl benzene sulfonyl chloride I, wherein R is C1-6 alkyl, H or F/Cl substituted C1-6 alkyl. The method comprises the steps of: (1) performing fluorine displacement reaction of 2,3-dichloro-trifluoromethylbenzene with KF or NaF in the presence of phase transfer catalyst to obtain compound of 2,3-difluoro-trifluoromethylbenzene, wherein the phase transfer catalyst is one or more selected from tetra-Me ammonium chloride, tetra-Me ammonium bromide, tetra-Et ammonium chloride, tetra-Ph phosphine chloride, hexamethyl guanidine chloride, etc., (2) performing reaction of the 2,3-difluoro-trifluoromethylbenzene with C1-C6 mercaptan, benzyl mercaptan or alkali metal salt thereof, benzyl mercaptan substituted with F, Cl, Br, nitro, or C1-C3 alkoxy, or alkali metal salt thereof, in the presence of acid-binding agent, to obtain the key intermediate, wherein the acid-binding agent is one or more of triethylamine, pyridine, NaH, NaOH, KOH, potassium acetate, etc., and (3) oxidizing and chlorinating with Cl2 to obtained intermediate, or reacting with C1-C6 alc. unsubstituted or substituted with F or Cl, or alkali metal salt thereof in the presence of catalyst, and then oxidizing and chlorinating with Cl2 to obtain aim products, wherein the catalyst is one or more of triethylamine, pyridine, sodium carbonate, potassium acetate, etc. The method has the advantages of easily available raw materials, simple process, high yield, and low cost. The experimental process involved the reaction of (2-Fluorophenyl)methanethiol(cas: 72364-46-6).Quality Control of (2-Fluorophenyl)methanethiol
The Article related to preparation substituted trifluoromethyl benzene sulfonyl chloride, Benzene, Its Derivatives, and Condensed Benzenoid Compounds: Sulfenic, Sulfinic, and Sulfonic Acids and Derivatives and other aspects.Quality Control of (2-Fluorophenyl)methanethiol
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