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ChemicalBook CAS DataBase List 2,3-dimethylbenzenethiol

2,3-dimethylbenzenethiol synthesis

3synthesis methods
-

Yield:18800-51-6 92%

Reaction Conditions:

with sodium tetrahydroborate;sodium hydroxide in water;acetonitrile at 80 - 82; for 3 h;Inert atmosphere;

Steps:

4 Example 4 Synthesis of compound of formula I (2,3-dimethylthiophenol)
134.2g (0.49mol) The bis(2,3-dimethylphenyl)disulfide prepared in Example 3 was dissolved in 500 mL acetonitrile and 50 mL water, Heat to reflux (80~82 °C) under nitrogen protection, At this temperature, 7.1g (0.19mol) NaBH4 dissolved in NaOH aqueous solution (52g mass fraction 45percent) was added dropwise, The dropping time is about 1 hour, and the reaction is continued for 2 hours. After the reaction was completed, acetonitrile was distilled off, and 200 ml of water was added at the same time. Cool to 60°C, add 400ml ethyl acetate, Add concentrated hydrochloric acid to adjust the pH to 1.5, separate the organic phase, Concentrate the ethyl acetate, 62.3 g of 2,3-dimethylthiophenol oily substance was obtained, The yield was 92.0percent, and the purity was 99.1percent.

References:

Puji Bio-technology (Taizhou) Co., Ltd.;Jia Qiang;Chen Xue;Miao Yingjie;Wang Yunzhong;Yang Jinjin;Ma Tianhua;Hua Ying;Xiong Chengtian;Wang Ru;Luo Xi;Fu Yongqian CN111187188, 2020, A Location in patent:Paragraph 0040-0042

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