benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetate/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetate/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetate/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetate/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 18 g m-chloroperbenzoic acid was added to 10 g benzyl 2,3,6,7-tetrahydro-1H-azepine-1-carboxylate in 250 ml dichloromethane at 0° C. in several portions. The mixture was allowed to warm to RT over 2 h. 1 L ethyl acetate was added and the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine. The organic layer was evaporated and the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5) to yield 10.4 g of the desired product. the solution was extracted with aqueous sodium bicarbonate, 1N aqueous sodium hydroxide and brine The organic layer was evaporated the residue was purified by chromatographie on silica gel (ethyl acetae/hexanes 1:5)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3 g benzyl 8-oxa-4-azabicyclo[5.1.0]octane-4-carboxylate in 70 mL 30% aqueous ammonia was stirred at 65° C. in a sealed vessel overnight. The reaction was extracted with dichloromethane. The organic layer was washed with brine, dried over sodium sulfate filtered and concentrated to yield 3.1 g of the desired product. (M+H)+: 265 The reaction was extracted with dichloromethane The organic layer was washed with brine dried over sodium sulfate filtered concentrated