HRID2265176

反应详情

EQUATION

反应方程式

HRID 2265176 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-(3,4-Dichloro-phenyl)-propionitrile (5.0 g, 25.0 mmol) was dissolved in THF (80 mL). BH3.THF (1 M in THF, 27.5 mL, 27.5 mmol) was added and the mixture was stirred overnight at rt. EtOH (10 mL) was added, the mixture was stirred for 20 min, and HCl in Et2O (2 M, 12.5 mL) was added. After stirring for 1 h, water was added, causing precipitation of the product. The product was collected by suction filtration and dried (4.2 g, 70%). MS (ESI+): mass calcd. for C9H11Cl2N, 204.1; m/z found, 205 [M+H]+. 1H NMR (400 MHz, CD3OD): 7.45-7.42 (m, 2H), 7.17-7.15 (m, 1H), 3.05-3.02 (m, 2H), 2.98-2.96 (m, 1H), 1.24 (d, J=6.5, 3H).

WORKUP

后处理

  1. stirringthe mixture was stirred for 20 min
  2. stirringAfter stirring for 1 h
  3. customprecipitation of the product
  4. filtrationThe product was collected by suction filtration
  5. customdried (4.2 g, 70%)