反应详情

A mixture of 5.85 parts of 6-(2-bromoethyl)-2,3,7-trimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one monohydrobromide, 4 parts of (4-fluorophenyl) (4-piperidinyl)methanone hydrochloride, 10 parts of sodium carbonate, 3 parts of a sodium methoxide solution 30% and 240 parts of 4-methyl-2-pentanone was stirred and refluxed for 20 hours using a water-separator. The reaction mixture was filtered hot over Hyflo and the filtrate was evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from a mixture of acetonitrile and 2,2'-oxybispropane (3:1 by volume) yielding 1 part of 6-[2-[4-(4-fluorobenzoyl)-1-piperidinyl]ethyl]-2,3,7-trimethyl-5H-thiazolo[3,2-a]pyrimidin-5-one; mp. 159.0° C. (compound 24).

1. temperaturerefluxed for 20 hours
2. filtrationThe reaction mixture was filtered hot over Hyflo
3. customthe filtrate was evaporated
4. customThe residue was purified by column-chromatography over silica gel using
5. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
6. customThe pure fractions were collected
7. customthe eluent was evaporated
8. customThe residue was crystallized from a mixture of acetonitrile and 2,2'-oxybispropane (3:1 by volume)