反应详情

A mixture of 47.6 parts of 1-(phenylmethyl)piperazine, 65,8 parts of 2-[4-(3-chloropropoxy)phenyl]-4,5-dihydrooxazole, 28.6 parts of sodium carbonate and 282 parts of N,N-dimethylformamide was stirred over weekend at 60°~65° C. The reaction mixture was evaporated and the residue was taken up in water. The product was extracted with dichloromethane. The extract was 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 converted into the (Z)-2-butenedioate salt in methanol. The salt was filtered off, washed with methanol and 2,2'-oxybispropane and crystallized from methanol. The product was filtered off, washed with water and dried at 70° C., yielding 40.6 parts (24.5%) of 1-[3-[4-(4,5-dihydro-2-oxazolyl)phenoxy]propyl]-4-(phenylmethyl)piperazine (Z)-2-butenedioate(1:2); mp. 178.0° C. (int. 15).

1. customThe reaction mixture was evaporated
2. extractionThe product was extracted with dichloromethane
3. customThe extract was dried
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
8. customThe pure fractions were collected
9. customthe eluent was evaporated
10. filtrationThe salt was filtered off
11. washwashed with methanol and 2,2'-oxybispropane
12. customcrystallized from methanol
13. filtrationThe product was filtered off
14. washwashed with water
15. customdried at 70° C.