반응 #75123

반응 방정식

1-chloro-4-methyl-2-nitrobenzene

3-amino-1-propanol

→

3-[(4-methyl-2-nitrophenyl)amino]-1-propanol

수율 33.0%

용매

butanol

반응 조건

후처리

1. 1
   온도refluxed for 30 hours
2. 2
   기타The reaction mixture is evaporated
3. 3
   workup.ADDITIONthe residue is poured onto water
4. 4
   추출The product is extracted with methylbenzene
5. 5
   세척The extract is washed with water and with a hydrochloric acid solution 2 N
6. 6
   기타dried
7. 7
   여과filtered
8. 8
   기타evaporated
9. 9
   기타The residue is purified by column-chromatography over silica gel using
10. 10
    workup.ADDITIONa mixture of trichloromethane and 5% of methanol as eluent
11. 11
    기타The pure fractions are collected
12. 12
    기타the eluent is evaporated

실험 절차

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.

출처