反应详情

3.7 g (15.9 mmol) of 7-benzyl-1-cyano-3-oxa-7-azabicyclo[3.3.0]octane in 5 ml of absolute tetrahydrofuran are added dropwise to a mixture of 1.5 g of lithium aluminium hydride in 100 ml of absolute tetrahydrofuran and the resulting mixture is heated under reflux for 15 hours. Decomposition is effected with 1.5 ml each of water, 15% strength sodium hydroxide solution, and again water, and the mixture is filtered with suction, and the aluminium salts are extracted by boiling on two occasions with 100 ml of tetrahydrofuran. The tetrahydrofuran solutions are concentrated and the residue is distilled. Yield: 3.2 g (86% of theory) Boiling point: 125°-130° C./0.04 mbar

1. temperaturethe resulting mixture is heated
2. temperatureunder reflux for 15 hours
3. filtrationthe mixture is filtered with suction
4. extractionthe aluminium salts are extracted
5. concentrationThe tetrahydrofuran solutions are concentrated
6. distillationthe residue is distilled