BUPIRIMATE synthesis

Yield:41483-43-6 94%

Reaction Conditions:

with 18-crown-6 ether;potassium carbonate in water;ethyl acetate for 2 h;Reflux;Reagent/catalyst;Solvent;

Steps:

1-10 Example 4
Put 20.9g of ethirimol,15.2g potassium carbonate, 180ml ethyl acetate, 0.018ml water, 0.2% 18-crown-6 were added to the reaction flask in sequence, heated to 50 with stirring, and 17.3g N,N-dimethylsulfonyl chloride was slowly added dropwise. After completion, the temperature was raised to reflux reaction for 2 hours, when the remaining 40% of the raw material was detected, hexamethylenetetramine was added to control the pH of the system to be 10, and the reaction was continued for 4 hours until the end. Then the system is cooled to 50°C, washed with water to adjust the system to neutrality, the water phase is separated, and the solvent is removed to obtain an oily substance. The solid is precipitated at a low temperature to 10°C, dried and weighed 29.7g, which is ethimphenol sulfonate , The yield is 94%, and the content is 97%.

References:

Xi'an Modern Chemical Institute;Wang Wei;Wang Lieping;Liu Kangyun;Huang Xiaoying;Zheng Xiaorui;Ning Binke;Xue Chao CN111303050, 2020, A Location in patent:Paragraph 0028-0050

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