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Benzoyl chloride, 2-chloro-4-(methylsulfonyl)- synthesis

3synthesis methods
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Yield:106904-10-3 97%

Reaction Conditions:

with dichlorosulfoxide;N,N-dimethyl-formamide in toluene at 0 - 50; for 27 h;

Steps:

1.5 5. 4- (methylsulfonyl) -2-chlorobenzoyl chlorideSynthesis

Four-necked flask add the compound 4- (methylsulfonyl) -2-chloro-benzoic acid 100g (0.426mol), toluene was added 500mL (not all dissolved at room temperature), add with stirring a catalytic amount of dimethylformamide 2mL. Installing a gas absorption device, was cooled to 0 deg.] C, slowly dropwise thionyl chloride 100g (0.84mol), was added dropwise need 3h, during the addition to maintain the temperature below 5 . After the dropwise addition, heated slowly to 50 (mixture was gradually clarified, and finally clear solution is formed), the reaction 24h, TLC detection reaction process (developing solvent: ethyl acetate). Rotary evaporation to remove the solvent and excess thionyl chloride to give a residue 105g, a yield of 97%, without further purification, was used directly in the next reaction.

References:

CN105693569,2016,A Location in patent:Paragraph 0054; 0055; 0056