反应详情

Twenty-five grams (0.56 mole) of N-(1-cyclohexyl-3-pyrrolidinyl)-p-nitro-N-methylbenzamide fumarate was partitioned between dil. sodium hydroxide and 400 ml. benzene. The benzene solution was dried with sodium sulfate and distilled to a volume of 250 ml. To this was added a finely ground mixture of 10 g. (0.045 mole) of phosphorous pentasulfide and 10 g. of potassium sulfide. The mixture was refluxed 4 hours and an additional 10 g. of phosphorous pentasulfide added and refluxed 2 hours. The benzene was decanted off of the hard solid. The solid was partitioned between dil. sodium hydroxide and chloroform. The chloroform was dried, concentrated and the residue crystallized twice from isopropyl ether-ethyl acetate. Yield 3.77 g. (19.5%); m.p. 108°-110°C.

1. dry with materialThe benzene solution was dried with sodium sulfate
2. distillationdistilled to a volume of 250 ml
3. additionTo this was added
4. additiona finely ground mixture of 10 g
5. temperatureThe mixture was refluxed 4 hours
6. temperaturerefluxed 2 hours
7. customThe benzene was decanted off of the hard solid
8. customThe solid was partitioned between dil. sodium hydroxide and chloroform
9. dry with materialThe chloroform was dried
10. concentrationconcentrated
11. customthe residue crystallized twice from isopropyl ether-ethyl acetate