HRID46845
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 171 parts of 1-chloro-4-methyl-2-nitrobenzene, 150 parts of 3-amino-1-propanol and 400 parts of butanol is stirred and refluxed for 30 hours. The reaction mixture is evaporated and the residue is poured onto water. The product is extracted with methylbenzene. The extract is washed with water and with a hydrochloric acid solution 2 N, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 5% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 70 parts (33%) of 3-[(4-methyl-2-nitrophenyl)amino]-1-propanol as a residue.
WORKUP
后处理
- temperaturerefluxed for 30 hours
- customThe reaction mixture is evaporated
- additionthe residue is poured onto water
- extractionThe product is extracted with methylbenzene
- washThe extract is washed with water and with a hydrochloric acid solution 2 N
- customdried
- filtrationfiltered
- customevaporated
- customThe residue is purified by column-chromatography over silica gel using
- additiona mixture of trichloromethane and 5% of methanol as eluent
- customThe pure fractions are collected
- customthe eluent is evaporated