HRID25084
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
- 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
- temperatureafter cooling it
- extractionextracted with dichloromethane
- concentrationThe organic layer was concentrated
- customthe residue was purified by column chromatography