反应详情

A mixture of 13.1 g. of p-cyanobenzaldehyde and 15 ml. of piperazine-1-carboxaldehyde was heated to 100° C. Over 10 minutes, 6 g. of 99% formic acid were added. The mixture was heated for 3 hours, then 200 ml. of 3.6 N hydrochloric acid in ethanol were added and the mixture was refluxed for 4 hours. The solid was collected, washed with ether and suspended in water. 10 N Sodium hydroxide extracted with three 100 ml. portions of chloroform and the combined extracts were evaporated. The residue was suspended in a mixture of 6 N hydrochloric acid and chloroform and filtered. The filtrate was adjusted to pH>7 with 10 N sodium hydroxide, extracted with chloroform, and the extract dried and evaporated to an oil which was distilled, giving α-(1-piperazinyl)-p-tolunitrile as a colorless liquid, b.p. 207°-209° C. (15 mm.).

1. additionA mixture of 13.1 g
2. temperatureThe mixture was heated for 3 hours
3. temperaturethe mixture was refluxed for 4 hours
4. customThe solid was collected
5. washwashed with ether
6. extraction10 N Sodium hydroxide extracted with three 100 ml
7. customportions of chloroform and the combined extracts were evaporated
8. additionThe residue was suspended in a mixture of 6 N hydrochloric acid and chloroform
9. filtrationfiltered
10. extractionextracted with chloroform
11. customthe extract dried
12. customevaporated to an oil which
13. distillationwas distilled