反应详情

温度

70 °C

A mixture of 74 parts of N-(2-hydroxy-1,1-dimethylethyl)-N'-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]thiourea and 360 parts of formic acid was stirred for 4 hours at 70° C. The reaction mixture was evaporated and the residue was dissolved in 260 parts of dichloromethane. The whole was neutralized with a sodium hydrogen carbonate solution. The precipitated product was filtered off, washed with water and dichloromethane and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol, saturated with ammonia, (99:1 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 4-methyl-2-pentanone. The product was filtered off and dried, yielding 44.1 parts (62.4%) of 4,5-dihydro-N-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-4,4-dimethyl-2-thiazolamine; mp. 232.0° C. (int. 8).

1. customThe reaction mixture was evaporated
2. dissolutionthe residue was dissolved in 260 parts of dichloromethane
3. filtrationThe precipitated product was filtered off
4. washwashed with water and dichloromethane
5. custompurified by column chromatography over silica gel using
6. additiona mixture of trichloromethane and methanol
7. customThe pure fractions were collected
8. customthe eluent was evaporated
9. customThe residue was crystallized from 4-methyl-2-pentanone
10. filtrationThe product was filtered off
11. customdried