反应详情

温度

100 °C

A mixture of 25 parts of 2-chloropropanenitrile, 61 parts of (4-fluorophenyl)(4-piperidinyl)methanone hydrochloride, 63 parts of sodium carbonate and 160 parts of acetonitrile is stirred and refluxed (100° C.) overnight. The reaction mixture is cooled, water is added and the layers are separated. The aqueous phase is extracted with 4-methyl-2-pentanone. The combined organic phases are dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane, hexane and methanol (50:49:1 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The solid residue is crystallized from 2,2'-oxybispropane. The product is filtered off, and dried yielding 17 parts of 4-(4-fluorobenzoyl)-α-methyl-1-piperidineacetonitrile; mp. 126.7° C.

1. temperatureThe reaction mixture is cooled
2. customthe layers are separated
3. extractionThe aqueous phase is extracted with 4-methyl-2-pentanone
4. customThe combined organic phases are dried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified by column-chromatography over silica gel using
8. additiona mixture of trichloromethane, hexane and methanol (50:49:1 by volume) as eluent
9. customThe pure fractions are collected
10. customthe eluent is evaporated
11. customThe solid residue is crystallized from 2,2'-oxybispropane
12. filtrationThe product is filtered off
13. customdried