HRID500548
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 title compound from example 27.1 (0.95 g, 3.7 mmol) and silver (1) carbonate (1.23 g, 4.48 mmol) were combined in a round bottom flask and purged with nitrogen. Toluene (10 mL) was added, followed by benzyl bromide (0.53 mL, 4.48 mmol) and the reaction was stirred for 72 h at room temperature. The silver salts were then removed by filtration through diatomaceous earth, which were then washed with dichloromethane. The filtrate was concentrated then purified by column chromatography on silica gel with 0-10% ethyl acetate in dichloromethane to give the title compound (off-white solid, 549 mg, 43
WORKUP
后处理
- custompurged with nitrogen
- additionToluene (10 mL) was added
- customThe silver salts were then removed by filtration through diatomaceous earth, which
- washwere then washed with dichloromethane
- concentrationThe filtrate was concentrated
- customthen purified by column chromatography on silica gel with 0-10% ethyl acetate in dichloromethane