HRID1510986

反应详情

EQUATION

反应方程式

HRID 1510986 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 10 ml Schlenk tube, 5.0 mg of dry zinc chloride was dissolved in 3.0 ml of absolute tetrahydrofuran and cooled to 0° C. under argon. Thereafter, 222 mg of (S)-2-trifluoromethanesulfonyloxypropionic acid (ee 99%) and 1.05 ml of n-butylmagnesium chloride (2.00 M solution in THF) were added in succession and the reaction was stirred for 3 h at 0° C. Thereafter, the reaction mixture was diluted with petroleum ether, saturated sodium carbonate solution was added and the organic phase was separated off. The aqueous phase was acidified with an aqueous 2 M HCl solution, saturated with NaCl and extracted 3 times with 10 ml of diethyl ether. The combined organic phases were dried over MgSO4 and concentrated in vacuo. Pure (S)-2-methylhexanoic acid (ee 99%) was obtained in 92% yield.

WORKUP

后处理

  1. additionwas added
  2. customthe organic phase was separated off
  3. extractionextracted 3 times with 10 ml of diethyl ether
  4. dry with materialThe combined organic phases were dried over MgSO4
  5. concentrationconcentrated in vacuo