HRID26380

反应详情

EQUATION

反应方程式

HRID 26380 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. After cooling, the autoclave was vented and the volatile constituents removed by evaporation in vacuo. The residue was taken up in ether and the ether solution was filtered to remove ammonium chloride which had precipitated. The ether filtrate was evaporated in vacuo to yield a solid product. The product was recrystallized from 95% 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
  3. customthe volatile constituents removed by evaporation in vacuo
  4. filtrationthe ether solution was filtered
  5. customto remove ammonium chloride which
  6. customhad precipitated
  7. customThe ether filtrate was evaporated in vacuo
  8. customto yield a solid product
  9. customThe product was recrystallized from 95% ethanol/ethyl acetate
  10. customto give 23.6 g