1-METHYL-1-CYCLOHEXANECARBOXYLIC ACID synthesis

Yield:1123-25-7 95.3%

Reaction Conditions:

at 10 - 40; for 2 h;

Steps:

1
In a 10 ml reaction flask, 98% 2-methylcyclohexanol (1) 11.68 (0.11] 1.01) was added and the temperature was reduced to 10 <€. Slowly dropping 98% chlorosulfonic acid 26.1 g (0.22mo 1 ), Dropping time lh temperature control at 10-15 ° C, drop finished, at 10-15 ° C, holding 30min, began dropping 98% formic acid 7.1 g (0.15mo 1), dropping time lh, dropping The temperature control in the process of 10-15 ° C, drop Bi, temperature, insulation temperature 35-40 ° C, insulation lh, then the reaction solution slowly into the 30g ice water, add 30ml toluene extraction, stirring 30min, Layered. The toluene layer was dried under reduced pressure to obtain 14.2 g of 1-methylcyclohexanecarboxylic acid product, 95.3% by titration and 95.3% yield.

References:

ZHEJIANG HETIAN CHEMICAL CO., LTD.;LIANYUNGANG HETIAN CHEMICAL CO., LTD.;HE, XIAOXIAO;YANG, JIANPING;ZHU, YAN;YANG, LINRONG CN106083572, 2016, A Location in patent:Paragraph 0019; 0020

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