HRID404665

反应详情

EQUATION

反应方程式

HRID 404665 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

2-(4-Chlorobutanamido)-2-phenylacetic acid (650 mg, 2.54 mmol) was dissolved in dry THF (8.5 ml) and the solution was cooled to 0° C. with an ice-bath stirring under nitrogen atmosphere. Potassium tert-butoxide (599 mg, 5.34 mmol) was added in three portions and a white suspension was obtained. The mixture was stirred at the same temperature for 15 minutes. 1N HCl was added dropwise till pH 2-3 and than the mixture was diluted with water (10 ml) and extracted three times with EtOAc (15 ml×3). The organic phase was dried (Na2SO4) and evaporated to obtain the title compound (352 mg, 63.2% yield) as a pale yellow spongy sticky solid.

WORKUP

后处理

  1. customa white suspension was obtained
  2. stirringThe mixture was stirred at the same temperature for 15 minutes
  3. extractionextracted three times with EtOAc (15 ml×3)
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. customevaporated