反应详情

Quinuclidinone (24.2 g, 0.19 mol) and 2,4,6-triisopropylbenzene sulphonohydrazide (72 g, 0.24 mol) (250 ml) were stirred together in anhydrous methanol for 3 hours. Potassium cyanide (33.8 g, 0.51 mol) was added and the mixture heated under reflux for 5 hours. The material isolated, after evaporation of the solvent, was partitioned between water and dichloromethane. The organic phase was dried (sodium sulphate) and evaporated and the residue fractionally distilled under reduced pressure to give 3-cyano-quinuclidine (6.1 g), approximate b.p. 95°-100° at 13 N.m-2 (0.1 mmHg).

1. temperaturethe mixture heated
2. temperatureunder reflux for 5 hours
3. customThe material isolated
4. customafter evaporation of the solvent
5. customwas partitioned between water and dichloromethane
6. dry with materialThe organic phase was dried (sodium sulphate)
7. customevaporated
8. distillationthe residue fractionally distilled under reduced pressure