HRID1672639
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
220 mg (0.53 mmol) of (2-{difluoro-[4′-(trifluoromethyl)biphenyl-4-yl]methoxy}-5-fluorophenyl)-methanol from Example 40A, 154 mg (0.59 mmol) of triphenylphosphine and 194.6 mg (0.59 mmol) tetrabromomethane are stirred in 5 ml dichloromethane at RT for 12 hours. 2 g of silica gel are added to the reaction mixture, and the mixture is then dried in vacuo and purified by silica gel chromatography (mobile phase: cyclohexane/ethyl acetate 10:1). 217 mg (0.46 mmol, 95% purity, 81% yield) of a solid are isolated.
WORKUP
后处理
- addition2 g of silica gel are added to the reaction mixture
- customthe mixture is then dried in vacuo
- custompurified by silica gel chromatography (mobile phase: cyclohexane/ethyl acetate 10:1)
- custom217 mg (0.46 mmol, 95% purity, 81% yield) of a solid are isolated