HRID2206930

反应详情

EQUATION

反应方程式

HRID 2206930 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(3,5-Dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidine (0.9 g) and 4-fluoro-2-(tri-fluoromethyl)benzonitrile (0.62 g) were weighed, dissolved in N,N-dimethylacetamide (10 ml), added with N,N-diisopropylethylamine (1.0 ml) at room temperature and reacted for 1 hour using a microwave reactor (trade name: INITIATOR™, manufactured by Biotage). The reaction solution was diluted by adding t-butyl methyl ether, and the organic layer was washed three times with water and then saturated brine in that order. The organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure and the residue obtained was purified by column chromatography to obtain 4-[3-(3,5-dichloro-4-fluorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-2-(trifluoromethyl)benzonitrile (1.1 g).

WORKUP

后处理

  1. customreacted for 1 hour
  2. additionThe reaction solution was diluted
  3. washthe organic layer was washed three times with water
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customthe residue obtained
  8. customwas purified by column chromatography