HRID500548

反应详情

EQUATION

反应方程式

HRID 500548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. custompurged with nitrogen
  2. additionToluene (10 mL) was added
  3. customThe silver salts were then removed by filtration through diatomaceous earth, which
  4. washwere then washed with dichloromethane
  5. concentrationThe filtrate was concentrated
  6. customthen purified by column chromatography on silica gel with 0-10% ethyl acetate in dichloromethane