反应详情

To a stirred mixture of 10 parts of 3-[(4,5-dichloro-2-nitrophenyl)amino]-1-propanol and 75 parts of trichloromethane are added dropwise 11.2 parts of sulfinyl chloride. Upon completion, stirring is continued for 4 hours at reflux temperature. The reaction mixture is evaporated and the residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from 2,2'-oxybispropane. The product is filtered off and dried, yielding 4,5-dichloro-N-(3-chloropropyl)-2-nitrobenzenamine; mp. 78° C.

1. temperatureat reflux temperature
2. customThe reaction mixture is evaporated
3. customthe residue is purified by column-chromatography over silica gel using
4. additiona mixture of trichloromethane and methanol (98:2) as eluent
5. customThe pure fractions are collected
6. customthe eluent is evaporated
7. customThe residue is crystallized from 2,2'-oxybispropane
8. filtrationThe product is filtered off
9. customdried