HRID1096678
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
To a solution of 2-hydroxy-5-methoxybenzaldehyde (0.152 g, 1.0 mmol) in dry MeCN (50 mL) was added 4-fluorobenzyl bromide (0.145 mg, 1.0 mmol), and anhydrous K2CO3 (0.27 g, 2.0 mmol). The mixture was refluxed under stirring for 4 h, and then evaporated in vacuo. Water (100 mL) was added and the mixture was extracted with EtOAc. The separated organic layer was dried with MgSO4, and then evaporated in vacuum. Finally, the residue was eluted through a silica gel column with n-hexane/EtOAc (4:1) to give white compound I (0.21 g, 88%).
WORKUP
后处理
- temperatureThe mixture was refluxed
- customevaporated in vacuo
- additionWater (100 mL) was added
- extractionthe mixture was extracted with EtOAc
- dry with materialThe separated organic layer was dried with MgSO4
- customevaporated in vacuum
- washFinally, the residue was eluted through a silica gel column with n-hexane/EtOAc (4:1)