HRID48101
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 (6-benzyloxy-naphthalen-2-yl)-methanol (17) (1 equi.) in CH2Cl2 (4 mL/mmole), a solution of phosphorus tribromide (4 mL/mmole), (0.4 equi.) was added at room temperature. The reaction mixture was stirred at that temperature for 24 h, quenched with water, extracted with dichloromethane, washed with brine, dried over MgSO4, and concentrated in vacuo. Purification by chromatography on silica gel (dichloromethane) and recrystallization from acetonitrile afforded 2-benzyloxy-6-bromomethyl-naphthalene (18) a white solid (92%).
WORKUP
后处理
- customquenched with water
- extractionextracted with dichloromethane
- washwashed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customPurification by chromatography
- customon silica gel (dichloromethane) and recrystallization from acetonitrile