HRID584684

反应详情

EQUATION

反应方程式

HRID 584684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 2-bromoaniline (2.18 g, 12.7 mmol) and 2,3-diphenylmaleic anhydride (3.17 g, (12.7 mmol) were stirred and heated under argon to 200° C. for 6 h. The mixture was cooled to room temperature, dissolved in CH2Cl2 (50 mL), dried (MgSO4) and evaporated. Purification of the crude product by flash chromatography on silica gel (5×25 cm column, 2 L of 3:7 hexanes/CH2Cl2, then CH2Cl2) gave first 4-(2-bromoanilino)-2,3-diphenyl-4-hydroxybutyrolactone (2.16 g, 40% yield) as a yellow solid, mp 162-164° C. and then the title compound as a bright yellow solid, mp 178-180° C., 2.00 g, 39% yield.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customPurification of the crude product by flash chromatography on silica gel (5×25 cm column, 2 L of 3:7 hexanes/CH2Cl2