HRID237556
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 cooled (0° C.) solution of 3-(4-bromo-3,5-dimethylphenoxy)-2,2-dimethylpropan-1-ol (251 mg) and triethylamine (160 μL) in dichloromethane (3 mL) is added methanesulfonyl chloride (75 μL). The mixture is stirred for 2 days while warming to room temperature. Then the mixture is diluted with dichloromethane, washed with saturated aqueous NaHCO3 solution and dried (MgSO4). The solvent is evaporated and the residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→50:50) to give the title compound. Yield: 271 mg; LC (method 7): tR=1.18 min; Mass spectrum (ESI+): m/z=365 [M+H]+.
WORKUP
后处理
- washwashed with saturated aqueous NaHCO3 solution
- dry with materialdried (MgSO4)
- customThe solvent is evaporated
- customthe residue is chromatographed on silica gel (cyclohexane/ethyl acetate 99:1→50:50)