HRID1873473

反应详情

EQUATION

反应方程式

HRID 1873473 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto give residual material
  3. washwashed with water
  4. dry with materiala saturated aqueous brine, subsequently dried over magnesium sulfate
  5. customAfter separating the drying agent
  6. filtrationby filtration
  7. distillationthe reaction liquor was distilled off under reduced pressure