HRID406821

反应详情

EQUATION

反应方程式

HRID 406821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of N-(5-formyl-2-methylphenyl)-4-(4-phenylquinazolin-2-ylamino)benzamide (250 mg, 0.546 mmol), cyclopropylamine (238 μL, 3.44 mmol), dichloromethane (10 m:), tetrahydrofuran (2 drops) and acetic acid (2 drops) was stirred at rt for 1 h. Sodium triacetoxyborohydride (275 mg, 1.30 mmol) was added and the mixture was stirred overnight. The crude reaction was diluted with dichloromethane, washed with saturated sodium bicarbonate and saturated sodium chloride and dried over sodium sulfate. The solution was concentrated on a rotary evaporator and purified by HPLC to give a yellow solid (143 mg, 52%).

WORKUP

后处理

  1. stirringthe mixture was stirred overnight
  2. customThe crude reaction
  3. washwashed with saturated sodium bicarbonate and saturated sodium chloride
  4. dry with materialdried over sodium sulfate
  5. concentrationThe solution was concentrated on a rotary evaporator
  6. custompurified by HPLC