HRID1672602

反应详情

EQUATION

反应方程式

HRID 1672602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an ice-cooled solution of 3-(trifluoromethyl)aniline (64.5 g, 0.40 mol) and triethylamine (60 ml) in acetone (700 ml) was added dropwise, ethyl 3-chloro-3-oxopropanoate (63.6 g, 0.42 mol) in acetone (50 ml). After the addition was complete (approx. 30 minutes), stirring was continued at RT overnight. The solvents were removed and water (1200 ml) was added. The resulting precipitate was filtered off, thoroughly washed twice with water and then dried to afford ethyl 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate as a yellow powder (109 g, 99%).

WORKUP

后处理

  1. additionwas added dropwise
  2. additionAfter the addition
  3. custom(approx. 30 minutes)
  4. customThe solvents were removed
  5. additionwater (1200 ml) was added
  6. filtrationThe resulting precipitate was filtered off
  7. washthoroughly washed twice with water
  8. customdried