反应详情

10.00 g (0.25 mol) of lithium aluminum hydride are introduced into 300 ml of absolute tetrahydrofuran and heated to reflux, and 18.00 g (50 mmol) of 7-benzyl-3-phenylsulfonyl-9-oxa-3,7-diazabicyclo[3.3.1]nonane, dissolved in 150 ml of absolute tetrahydrofuran, are added dropwise. The mixture is boiled under reflux for 48 hours, 10 ml portions of water, 15% strength potassium hydroxide solution and again water are added dropwise, and the organic salts are filtered off with suction and extracted by boiling twice with tetrahydrofuran. The tetrahydrofuran solutions are concentrated, and the residue is distilled under high vacuum. 5.30 g (43.5% of theory) of the product are obtained

1. temperatureheated
2. temperatureto reflux
3. additionare added dropwise
4. temperatureunder reflux for 48 hours
5. filtrationthe organic salts are filtered off with suction
6. extractionextracted
7. concentrationThe tetrahydrofuran solutions are concentrated
8. distillationthe residue is distilled under high vacuum
9. custom5.30 g (43.5% of theory) of the product are obtained