反应详情

To a solution of 3-benzyl-8-methyl-3,8-diazabicyclo[3.2.1]octane-2,4-dione (28.3 g; 0.116 mol) in 200 ml of absolute dioxane LiAlH4 (7.6 g; 0.2 mol) was added and the mixture boiled under argon for 18 hours. Then a mixture of water (7.5 ml) and dioxane (40 ml) was added drop-wise to the reaction mixture. The suspension was mixed for 20 minutes and filtered trough a dense glass filter. The filtrate was evaporated and the residue was distilled on Büchi oven for distillation at 120° C. and 0.1 mbar. Yield 17.6 g (70%).

1. additionwas added drop-wise to the reaction mixture
2. additionThe suspension was mixed for 20 minutes
3. filtrationfiltered trough a dense glass
4. filtrationfilter
5. customThe filtrate was evaporated
6. distillationthe residue was distilled on Büchi oven for distillation at 120° C.