HRID25084

反应详情

EQUATION

反应方程式

HRID 25084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 3.0 g (7.82 mmol) of the starting material XXIV and 15 ml of acetic anhydride was stirred at 110° C. for 1 h, then after cooling it was diluted with water and extracted with dichloromethane. The organic layer was concentrated and the residue was purified by column chromatography using silica gel (MN Kieselgel 60) as adsorbent and a mire of n-hexane-ethyl acetate (2:1) as eluent to yield 1.58 g (50%) of the title compound; Mp.: 191-200° C.

WORKUP

后处理

  1. temperatureafter cooling it
  2. extractionextracted with dichloromethane
  3. concentrationThe organic layer was concentrated
  4. customthe residue was purified by column chromatography