HRID1971217

反应详情

EQUATION

反应方程式

HRID 1971217 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

18 g (62.6 mmol) of 6-bromo-4-chloro-3-nitro-quinoline (Example 1c) and 11 g (68.9 mmol) of (2-(4-amino-phenyl)-2-methyl-propionitrile (Example 1e) are dissolved in 350 ml of acetic acid and stirred for 2 h. After this time, water is added and the yellow precipitate is filtered off and washed with H2O. The solid is dissolved in EtOAc-THF (1:1), washed with sat. aqueous NaHCO3 and dried over MgSO4. The organic phase is evaporated to dryness to give the title compound as a yellow solid. ES-MS: 411, 413 (M+H)+, Br pattern; analytical HPLC: tret=3.69 min (Grad 1).

WORKUP

后处理

  1. filtrationthe yellow precipitate is filtered off
  2. washwashed with H2O
  3. dissolutionThe solid is dissolved in EtOAc-THF (1:1)
  4. washwashed with sat. aqueous NaHCO3
  5. dry with materialdried over MgSO4
  6. customThe organic phase is evaporated to dryness