HRID26380
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe autoclave was sealed
- temperatureAfter cooling
- customthe volatile constituents removed by evaporation in vacuo
- filtrationthe ether solution was filtered
- customto remove ammonium chloride which
- customhad precipitated
- customThe ether filtrate was evaporated in vacuo
- customto yield a solid product
- customThe product was recrystallized from 95% ethanol/ethyl acetate
- customto give 23.6 g