HRID1249363
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
PROCEDURE
实验过程
A mixture of 20 parts of 4-chloro-α-(2-chloro-4-nitrophenyl)-α-methylbenzeneacetonitrile, 7 parts of iron powder, 250 parts of ammonium chloride solution 0.78N and 200 parts of methylbenzene was stirred and refluxed for 3 hours. The reaction mixture was filtered hot. The aqueous phase was separated and washed with methylbenzene. The combined organic layers were washed successively with water, sodium hydrogen carbonate solution and again with water, dried and evaporated. The residue was washed with 1,1'-oxybisethane and dried, yielding 10 parts of α-(4-amino-2-chlorophenyl)-4-chloro-α-methylbenzeneacetonitrile; mp. 135.2° C. (intermediate 24).
WORKUP
后处理
- temperaturerefluxed for 3 hours
- filtrationThe reaction mixture was filtered hot
- customThe aqueous phase was separated
- washwashed with methylbenzene
- washThe combined organic layers were washed successively with water, sodium hydrogen carbonate solution and again with water
- customdried
- customevaporated
- washThe residue was washed with 1,1'-oxybisethane
- customdried