反应详情

A solution of 29.6 parts of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide and 14.9 parts of 4-fluoro-2-methylbenzeneacetonitrile in 90 parts of methylbenzene is added dropwise to a solution of 5.6 parts of lithium amide in 270 parts of methylbenzene at about 90° C. Upon completion, the whole is heated to reflux and stirred overnight at reflux temperature. The reaction mixture is cooled, poured onto water and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is crystallized from 2-propanol, yielding 27 parts (72.6%) of 4-(4-fluoro-2-methylphenyl)-1-(4-methylphenylsulfonyl)-4-piperidinecarbonitrile.

1. temperatureUpon completion, the whole is heated
2. temperatureto reflux
3. temperatureat reflux temperature
4. temperatureThe reaction mixture is cooled
5. additionpoured onto water
6. customthe layers are separated
7. customThe organic phase is dried
8. filtrationfiltered
9. customevaporated
10. customThe residue is crystallized from 2-propanol