tert-butyl 2,3,3a,4,6,6a-hexahydro-1H-pyrrolo[3,4-c]pyrrole-5-carboxylate;hydrochloride

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

実験手順: tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate hydrochloride (10 g, 0.04 mol; see Preparation A above) and triethylamine (14 mL, 0.1 mol) were mixed in CHCl3 (100 mL). N-benzyloxy-carbonyloxy succinimide (11 g, 0.044 mol), dissolved in CHCl3 (100 mL), was added at 0–5° C. The mixture was allowed to slowly reach room temperature and was stirred at rt for 5 h. The reaction mixture was washed with water, dried (Na2SO4) and evaporated, giving the sub-title compound in quantitative yield. was added at 0–5° C was allowed to slowly reach room temperature The reaction mixture was washed with water dried (Na2SO4) evaporated

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

実験手順: To a solution of 3-benzyl-7-(tert-butoxycarbonyl)-3,7-diazabicyclo[3.3.0]-octane hydrochloride (91.1 g, 269 mmol; from step (d) above) in methanol (250 mL) under a N2 atmosphere there was added 10% Pd/C (w/w; 9.8 g). The N2 atmosphere was exchanged for H2 (1 atm of pressure) and the reaction was stirred for 18 h. The reaction was filtered through a pad of cellulose to remove the catalyst. The filtrate was concentrated in vacuo to afford an off-white solid. The solid was slurried in EtOAc and collected. After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there was obtained 58.0 g (87%) of the title compound as an off-white solid. The reaction was filtered through a pad of cellulose to remove the catalyst The filtrate was concentrated in vacuo to afford an off-white solid collected After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there

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

実験手順: To a solution of 3-benzyl-7-(tert-butoxycarbonyl)-3,7-diazabicyclo[3.3.0]-octane hydrochloride (91.1 g, 269 mmol; from step (d) above) in methanol (250 mL) under a N2 atmosphere there was added 10% Pd/C (w/w; 9.8 g). The N2 atmosphere was exchanged for H2 (1 atm of pressure) and the reaction was stirred for 18 h. The reaction was filtered through a pad of cellulose to remove the catalyst. The filtrate was concentrated in vacuo to afford an off-white solid. The solid was slurried in EtOAc and collected. After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there was obtained 58.0 g (87%) of the title compound as an off-white solid. The reaction was filtered through a pad of cellulose to remove the catalyst The filtrate was concentrated in vacuo to afford an off-white solid collected After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there

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

実験手順: tert-Butyl hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate hydrochloride (10 g, 0.04 mol; see Preparation A above) and triethylamine (14 mL, 0.1 mol) were mixed in CHCl3 (100 mL). N-benzyloxy-carbonyloxy succinimide (11 g, 0.044 mol), dissolved in CHCl3 (100 mL), was added at 0–5° C. The mixture was allowed to slowly reach room temperature and was stirred at rt for 5 h. The reaction mixture was washed with water, dried (Na2SO4) and evaporated, giving the sub-title compound in quantitative yield. was added at 0–5° C was allowed to slowly reach room temperature The reaction mixture was washed with water dried (Na2SO4) evaporated

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

実験手順: To a solution of 3-benzyl-7-(tert-butoxycarbonyl)-3,7-diazabicyclo[3.3.0]-octane hydrochloride (91.1 g, 269 mmol; from step (d) above) in methanol (250 mL) under a N2 atmosphere there was added 10% Pd/C (w/w; 9.8 g). The N2 atmosphere was exchanged for H2 (1 atm of pressure) and the reaction was stirred for 18 h. The reaction was filtered through a pad of cellulose to remove the catalyst. The filtrate was concentrated in vacuo to afford an off-white solid. The solid was slurried in EtOAc and collected. After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there was obtained 58.0 g (87%) of the title compound as an off-white solid. The reaction was filtered through a pad of cellulose to remove the catalyst The filtrate was concentrated in vacuo to afford an off-white solid collected After drying in a vacuum oven for 18 h at 60° C./66.5 Pa (0.5 mm Hg) there