HRID1606559

反应详情

EQUATION

反应方程式

HRID 1606559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

An alternative procedure is as follows. A mixture of 4-trifluoromethylacetophenone (18.8 g) glyoxylic acid monohydrate (18.8 g), Ac2O (20 ml) and a drop of Et3N was heated to 135°, internal temperature. More Et3N (2 ml) was added, and the mixture was held at 135° for 20 minutes. The mixture was cooled and evaporated to dryness in vacuo. The solid residue was digested with H2O, filtered, dried and recrystallized from C6H6 to give the title compound, 12.2 g (50%), mp 149°-151°.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. customevaporated to dryness in vacuo
  3. filtrationfiltered
  4. customdried
  5. customrecrystallized from C6H6