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
A solution of 2-bromo-4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]benzyl methanesulfonate (1.0 g) in THF (5 ml) was added dropwise to a mixed solution of aqueous ammonia (30%, 30 ml), methanol (30 ml) and THF (30 ml), and the reaction mixture was stirred for 20 hours at room temperature. The mixture was concentrated under reduced pressure to give residual material. The residue was dissolved with t-butyl methyl ether and washed with water and a saturated aqueous brine, subsequently dried over magnesium sulfate. After separating the drying agent by filtration, the reaction liquor was distilled off under reduced pressure, to obtain 1-{2-bromo-4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)-3,4-dihydro-2H-pyrrol-5-yl]phenyl}methanamine (0.8 g).
WORKUP
后处理
- concentrationThe mixture was concentrated under reduced pressure
- customto give residual material
- washwashed with water
- dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
- customAfter separating the drying agent
- filtrationby filtration
- distillationthe reaction liquor was distilled off under reduced pressure