HRID1428720

反应详情

EQUATION

反应方程式

HRID 1428720 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of tert-butyl (2-(3-chloro-4-fluorophenyl)-6-(trifluoromethyl)pyridin-3-yl)methylcarbamate (5.27 g, 13.04 mmol) in 1,4-dioxane (5 mL) was added with 1,4-dioxane.HCl (10 mL) under cooling and the reaction mixture was allowed to stir for 12 h. The reaction mixture was concentrated under reduced pressure and was co-distilled with methanol thrice and the solid obtained was filtered through sintered funnel and was washed with 10% ethyl acetate in n-hexane to afford pure (2-(3-chloro-4-fluorophenyl)-6-(trifluoromethyl)pyridin-3-yl)methanamine hydrochloride (4.14 g, 93%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe solid obtained
  3. filtrationwas filtered through sintered funnel
  4. washwas washed with 10% ethyl acetate in n-hexane