HRID46699

反应详情

EQUATION

反应方程式

HRID 46699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Fifty grams (0.27 mole) of 4-chloro-3-nitrobenzyl alcohol, 250 ml. of methanol and 200 ml. of liquid ammonia were loaded into a cold autoclave. The autoclave was sealed and heated to a temperature of 150° C. The reaction was continued for 6 hours. After cooling the autoclave was vented and the reaction mixture was evaporated in vacuo. The residue was taken up in ether and the ether solution was filtered to separate the ammonium chloride. The ether filtrate was evaporated in vacuo to yield a solid product. The product was recrystallized from 2-B ethanol/ethyl acetate to give 23.6 g. (52 percent yield) of 4-amino-3-nitrobenzyl alcohol, mp. 100°-101° C.

WORKUP

后处理

  1. customThe autoclave was sealed
  2. temperatureAfter cooling the autoclave
  3. customthe reaction mixture was evaporated in vacuo
  4. filtrationthe ether solution was filtered
  5. customto separate the ammonium chloride
  6. customThe ether filtrate was evaporated in vacuo
  7. customto yield a solid product
  8. customThe product was recrystallized from 2-B ethanol/ethyl acetate
  9. customto give 23.6 g