HRID1967416
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe reaction mixture was stirred for an hour
- filtrationA precipitate was filtrated
- filtrationThe precipitate which was filtrated
- dissolutionwas dissolved in methylene chloride again
- customthe solution was purified by column chromatography on silica gel (ethyl acetate:n-hexane=1:3)