反应详情

A mixture of 6.4 parts of sodium carbonate and 120 parts of 4-methyl-2-pentanone is stirred and refluxed with water-separator. Then there are added 4.1 parts of N-[4-(methoxymethyl)-4-piperidinyl]-N-phenylpropanamide and 5.5 parts of [2-(1-naphthalenyl)ethyl]4-methylbenzenesulfonate and the whole is stirred and refluxed for 20 hours. The reaction mixture is cooled to room temperature and poured onto water. The organic phase is separated, washed with water, dried, filtered and evaporated. The oily residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and 7% of methanol as eluent. The pure fractions are collected and the eluent is evaporated. The oily residue solidifies on triturating in hexane. The product is filtered off and crystallized from a small amount of 2,2'-oxybispropane, yielding 2.8 parts (43.4%) of N-{4-(methoxymethyl)-1-[2-(1-naphthalenyl)ethyl]-4-piperidinyl}-N-phenylpropanamide; mp. 109.8° C.

1. stirringthe whole is stirred
2. temperaturerefluxed for 20 hours
3. additionpoured onto water
4. customThe organic phase is separated
5. washwashed with water
6. customdried
7. filtrationfiltered
8. customevaporated
9. customThe oily residue is purified by column-chromatography over silica gel using
10. additiona mixture of trichloromethane and 7% of methanol as eluent
11. customThe pure fractions are collected
12. customthe eluent is evaporated
13. customon triturating in hexane
14. filtrationThe product is filtered off
15. customcrystallized from a small amount of 2,2'-oxybispropane