HRID48235
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
PROCEDURE
实验过程
The product from Example 89 (0.14 g, 0.5 mmol) was solubilized in a minimal amount of dimethylformamide and then treated with 2 mL dichloromethane, acetic anhydride (0.15 g) and triethylamine (0.15 g). After the mixture stirred at room temperature for 18 h, it was poured onto dichloromethane/water. The aqueous layer was washed with dichloromethane and the combined organic layers over sodium sulfate, filtered and evaporated to give a dark syrup. The syrup was purified by silica gel chromatography (ethyl acetate as eluant) to give the title compound (30 mg, 19% yield).
WORKUP
后处理
- additionit was poured onto dichloromethane/water
- washThe aqueous layer was washed with dichloromethane
- filtrationthe combined organic layers over sodium sulfate, filtered
- customevaporated
- customto give a dark syrup
- customThe syrup was purified by silica gel chromatography (ethyl acetate as eluant)