HRID394756

反应详情

EQUATION

反应方程式

HRID 394756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 2-chloro-3-nitrobenzamide (1.02 g, 4.9 mmol) in P2O5/(TMS)2O/1,2-dichloroethane (30 mL) was heated at 85° C. for 18 hours. After it was cooled to 25° C., the solution was filtered through a plug of silica gel (60 mL), eluting with 5% methanol/CHCl3 (400 mL). The combined washes were concentrated under reduced pressure to give 2-chloro-3-nitrobenzonitrile as an off-white solid (0.66 g, 74%).

WORKUP

后处理

  1. filtrationthe solution was filtered through a plug of silica gel (60 mL)
  2. washeluting with 5% methanol/CHCl3 (400 mL)
  3. concentrationThe combined washes were concentrated under reduced pressure