反应详情

A mixture of 6.8 parts of 6-(2-bromoethyl)-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one, 3.15 parts of α-(4-fluorophenyl)-4-piperidinemethanol, 4.8 parts of sodium carbonate, 0.1 parts of potassium iodide and 200 parts of 4-methyl-2-pentanone was stirred and refluxed for 24 hours. The reaction mixture was cooled, washed with 50 parts of water, dried, filtered and evaporated. The residue was purified by columnchromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue solidified upon triturating in acetonitrile. The product was filtered off, washed twice with acetonitrile and dried, yielding 2.5 parts (42%) of 6-[2-[4-[(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-2,3-dihydro-7-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one; mp. 204.3° C. (compound 33).

1. temperaturerefluxed for 24 hours
2. temperatureThe reaction mixture was cooled
3. washwashed with 50 parts of water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by columnchromatography over silica gel using
8. additiona mixture of trichloromethane and methanol (90:10 by volume) as eluent
9. customThe pure fractions were collected
10. customthe eluent was evaporated
11. customupon triturating in acetonitrile
12. filtrationThe product was filtered off
13. washwashed twice with acetonitrile
14. customdried