反应详情

To a stirred and warmed (30°-40° C.) solution of 72 parts of N-[1-(1-methylethyl)-4-piperidinylidene]benzeneamine in 480 parts of methanol are added portionwise 20 parts of sodium borohydride. Upon completion, stirring is continued overnight at at room temperature. The reaction mixture is evaporated and the residue is dissolved in water. The solution is extracted with 4-methyl-2-pentanone. The extract is washed with water and acidified with a diluted hydrochloric acid solution. The aqueous acid phase is alkalized with a diluted sodium hydroxide solution till pH 9 and the product is extracted with 4-methyl-2-pentanone. The extract is washed with water, dried, filtered and evaporated. The residue is distilled (bp. 135°-140° C. at 0.2 mm. pressure) and the distillate is crystallized from petroleumether, yielding 21 parts of 1-(1-methylethyl)-N-phenyl-4-piperidinamine; mp. 69.3° C.

1. stirringUpon completion, stirring
2. customThe reaction mixture is evaporated
3. dissolutionthe residue is dissolved in water
4. extractionThe solution is extracted with 4-methyl-2-pentanone
5. washThe extract is washed with water
6. extractionthe product is extracted with 4-methyl-2-pentanone
7. washThe extract is washed with water
8. customdried
9. filtrationfiltered
10. customevaporated
11. distillationThe residue is distilled (bp. 135°-140° C. at 0.2 mm. pressure)
12. customthe distillate is crystallized from petroleumether