3-Methyl-8-quinolinesulphonyl chloride synthesis

Yield:74863-82-4 178 g

Reaction Conditions:

with bis(trichloromethyl) carbonate;triethylamine in toluene at 25 - 40; for 3 h;Reagent/catalyst;Temperature;

Steps:

1-6 Example 1:
The above reaction mixture was cooled to 25 ° C, and a solution of bis(trichloromethyl)carbonate (103.8 g, 0.35 mol) in toluene (500 mL) was added. Under ice water conditions, triethylamine (50.5 g, 0.5 mol) was added dropwise to the reaction bottle, and the reaction was completed for 1 hour. The reaction mixture was slowly warmed to 40 ° C and reacted for 2 hours. Cool, add cold water (500 mL), separate the toluene solution, wash with water, and concentrate to obtain the crude product. Toluene was recrystallized to obtain off-white crystals (178g) with a yield of 74%. The content of 3-methylquinoline-8-sulfonyl chloride analyzed by liquid chromatography was 99.41%.

References:

Beijing Chengyu Chemical Co., Ltd.;Song Ye CN110872252, 2020, A Location in patent:Paragraph 0046-0049; 0058-0077

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