HRID1042258

反应详情

EQUATION

反应方程式

HRID 1042258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(6-bromo-7-methyl-8-nitroquinazolin-4-ylamino)benzonitrile (400 mg, 1.04 mmol) and Pd/C (10%˜30 mg) in EtOH (20 mL) was stirred under H2 gas (1 atm) overnight. 30 mL of NH3/MeOH (2 M) was added and the mixture was filtered through celite and washed with MeOH/DCM (˜1:1). After removal of solvent the product was purified by flash chromatography eluting with MeOH/DCM (1-5%) to give 4-(8-amino-7-methylquinazolin-4-ylamino)benzonitrile (238 mg, 83%). MS (ESI, pos. ion) m/z: 276 [M+H]+

WORKUP

后处理

  1. filtrationthe mixture was filtered through celite
  2. washwashed with MeOH/DCM (˜1:1)
  3. customAfter removal of solvent the product
  4. customwas purified by flash chromatography
  5. washeluting with MeOH/DCM (1-5%)