HRID1942630

反应详情

EQUATION

反应方程式

HRID 1942630 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 2-isobutyl-5-nitrobenzonitrile (D56) (7.5 g) in methanol (80 mL) and water (80 mL) was added ammonium formate (51.9 g) and zinc (26.9 g). The reaction mixture was stirred at 80° C. for 4 h. After cooling the reaction, the solid was filtered, the filtrate was concentrated under reduced pressure, the residue was extracted with EtOAc (300 mL*2), the combined organic layers were washed with water (30 mL*2), dried and concentrated to give 5-amino-2-(2-methylpropyl)benzonitrile (D57) (17.5 g) as a colorless solid. MS (ES): C11H14N2 requires 174. found 175.1 (M+H+).

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe reaction
  3. filtrationthe solid was filtered
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. extractionthe residue was extracted with EtOAc (300 mL*2)
  6. washthe combined organic layers were washed with water (30 mL*2)
  7. customdried
  8. concentrationconcentrated