反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Hereinafter, the present invention is explained in more detail below referring to production example and reference examples but the present invention should not be limited in the following examples. Example 1 (preparation example of the present compound) A mixture solution of 27.5 g of ethyl 3,3-dimethyl-4,6,6-trichloroheptanoate and 204 g of a 20% ethanol solution of sodium ethoxide was stirred under reflux for 48 hours. The reaction solution was poured into ice and extracted with 500 ml of ethyl acetate 3 times. The combined extract was washed with 500 ml of water twice, dried over anhydrous sodium sulfate, concentrated under reduced pressure and the residue was distilled under reduced pressure to afford 11.6 g of ethyl trans-3-(1-propynyl)-2,2-dimethylcyclopropanecarboxylate (yield: 64%).
WORKUP
后处理
- temperatureunder reflux for 48 hours
- additionThe reaction solution was poured into ice
- extractionextracted with 500 ml of ethyl acetate 3 times
- extractionThe combined extract
- washwas washed with 500 ml of water twice
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- distillationthe residue was distilled under reduced pressure