HRID1967416

反应详情

EQUATION

反应方程式

HRID 1967416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Ammonium acetate (92.5 g) was added to the acetic acid solution (430 mL) of the compound prepared in Example 16 under argon gas atmosphere. The reaction mixture was stirred at 100° C. for an hour. Water was added to the reaction mixture, and the reaction mixture was stirred for an hour. A precipitate was filtrated. The precipitate which was filtrated was dissolved in methylene chloride again, and the solution was purified by column chromatography on silica gel (ethyl acetate:n-hexane=1:3) to obtain a title compound (44.1 g) having the following physical data.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for an hour
  2. filtrationA precipitate was filtrated
  3. filtrationThe precipitate which was filtrated
  4. dissolutionwas dissolved in methylene chloride again
  5. customthe solution was purified by column chromatography on silica gel (ethyl acetate:n-hexane=1:3)