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
In an argon atmosphere, a mixture of 6.55 g (39.7 mmol) of 15, 10.9 g (79.3 mmol) of K2CO3, 1.0 g (5.94 mmol) of KI and 80 mL of anhydrous DMF was stirred for 10 min at room temperature. After that 7.52 g (59.5 mmol) of benzyl chloride was added in one portion. The resulting mixture was stirred for 2 hr at 70° C. and then evaporated to dryness. To the residue, 70 mL of water and 30 mL of dichloromethane were added. The organic layer was separated, and the aqueous layer was washed by 2×50 mL of dichloromethane. The combined organic extract was dried over Na2SO4 and then evaporated to dryness. The residue was washed by 50 mL of cold ether and dried in vacuum. Yield 9.71 g (96%) of a white solid.
WORKUP
后处理
- stirringThe resulting mixture was stirred for 2 hr at 70° C.
- customevaporated to dryness
- additionTo the residue, 70 mL of water and 30 mL of dichloromethane were added
- customThe organic layer was separated
- washthe aqueous layer was washed by 2×50 mL of dichloromethane
- extractionThe combined organic extract
- dry with materialwas dried over Na2SO4
- customevaporated to dryness
- washThe residue was washed by 50 mL of cold ether
- customdried in vacuum