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2-Chloro-2'-methylbenzophenone synthesis

9synthesis methods
-

Yield:4888-03-3 92.5%

Reaction Conditions:

Stage #1: 2-methylchlorobenzenewith iodine;magnesium in diethyl ether; for 4 h;Inert atmosphere;
Stage #2: o-chlorobenzoyl chloride in 5,5-dimethyl-1,3-cyclohexadiene;diethyl ether; for 36 h;Cooling with ice;Reflux;

Steps:

2.1; 2.2 (1) Preparation of format reagent

48 g (2.0 M) of magnesium powder was taken, placed in a four-neck round bottom flask, and dried with hot nitrogen gas, and cooled for 30 minutes. plusInto the o-methyl chlorobenzene, a small amount of ether, iodine, heating to initiate the reaction. Diethyl ether was added dropwise to the reaction flask to make a total solvent amount of 1000 ml.The reaction temperature was controlled, reacted for 4 hours, cooled, and the resulting format reagent was used.(2) Preparation of intermediate 6-(2-chlorobenzoyl)tolueneFormat the reagent in diethyl ether solution (concentration 2.0M) 1000 ml, slowly drip into the ice bath containing 420.0 g(2.4 M) o-chlorobenzoyl chloride in xylene solution, the reflux reaction was continued for 36 hours, the reaction was completed, and the solvent was evaporated under reduced pressure. anti-The contents were poured into 1000 ml of ice-dilute hydrochloric acid, extracted twice with 1000 ml of toluene, and toluene was combined. Dry anhydrous magnesium sulfate, minusThe toluene was distilled off to give an intermediate 6-(2-chlorobenzoyl)toluene (425.6 g, yield: 92.5%).

References:

CN108530293,2018,A Location in patent:Paragraph 0041; 0042; 0044; 0045; 0046; 0047

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