反应详情

To 75 parts of a hydrobromic acid solution 48% in water was added a small amount of sodium hydrogen sulfite. Then there were added 1.7 parts of N-butyl-N-(3-hydroxypropyl)-N'-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]thiourea. The whole was stirred and refluxed for 3 hours. The reaction mixture was evaporated. The residue was dissolved in a mixture of methanol and water. The solution was neutralized with a sodium hydrogen carbonate solution. The product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 0.6 parts (38%) of 4-[4-[4-[(3-butyltetrahydro-1,3-thiazin-2-ylidene)amino]phenyl]-1-piperazinyl]phenol; mp. 143.0° C. (45).

1. temperaturerefluxed for 3 hours
2. customThe reaction mixture was evaporated
3. dissolutionThe residue was dissolved in a mixture of methanol and water
4. extractionThe product was extracted with dichloromethane
5. washThe extract was washed with water
6. customdried
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by column chromatography over silica gel using
10. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
11. customThe pure fractions were collected
12. customthe eluent was evaporated
13. customThe residue was crystallized from 2-propanol
14. filtrationThe product was filtered off
15. customdried