1-ISOPROPYL-PYRROLIDIN-3-YLAMINE DIHYDROCHLORIDE

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

実験手順: t-Butyl-1-isopropylpyrrolidin-3-ylcarbamate (0.90 g, 3.9 mmol) obtained in Preparation Example (2-vii-1) was dissolved in dichloromethane (10 ml) in a 50 ml vessel, and trifluoroacetic acid (1.45 ml, 1.95 mmol, 5 eq.) was slowly added dropwise thereto while stirring. The resulting mixture was reacted for 18 hrs. After the completion of reaction, the reaction mixture was distilled and concentrated under reduced pressure, and then subjected to azeotropic distillation with CHCl3 3 times. The resultant was basified with aqueous 2N potassium hydroxide solution (20 ml) and extracted with CHCl3 3 times. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, filtered and distilled under reduced pressure to obtain 433 mg of the title compound as yellow oil (yield 86%). The resulting mixture was reacted for 18 hrs After the completion of reaction the reaction mixture was distilled concentrated under reduced pressure subjected to azeotropic distillation with CHCl3 3 times extracted with CHCl3 3 times The organic layer was separated washed with brine dried over anhydrous magnesium sulfate filtered distilled under reduced pressure

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

実験手順: t-Butyl-1-isopropylpyrrolidin-3-ylcarbamate (0.90 g, 3.9 mmol) obtained in Preparation Example (2-vii-1) was dissolved in dichloromethane (10 ml) in a 50 ml vessel, and trifluoroacetic acid (1.45 ml, 1.95 mmol, 5 eq.) was slowly added dropwise thereto while stirring. The resulting mixture was reacted for 18 hrs. After the completion of reaction, the reaction mixture was distilled and concentrated under reduced pressure, and then subjected to azeotropic distillation with CHCl3 3 times. The resultant was basified with aqueous 2N potassium hydroxide solution (20 ml) and extracted with CHCl3 3 times. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, filtered and distilled under reduced pressure to obtain 433 mg of the title compound as yellow oil (yield 86%). The resulting mixture was reacted for 18 hrs After the completion of reaction the reaction mixture was distilled concentrated under reduced pressure subjected to azeotropic distillation with CHCl3 3 times extracted with CHCl3 3 times The organic layer was separated washed with brine dried over anhydrous magnesium sulfate filtered distilled under reduced pressure

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

実験手順: t-Butyl-1-isopropylpyrrolidin-3-ylcarbamate (0.90 g, 3.9 mmol) obtained in Preparation Example (2-vii-1) was dissolved in dichloromethane (10 ml) in a 50 ml vessel, and trifluoroacetic acid (1.45 ml, 1.95 mmol, 5 eq.) was slowly added dropwise thereto while stirring. The resulting mixture was reacted for 18 hrs. After the completion of reaction, the reaction mixture was distilled and concentrated under reduced pressure, and then subjected to azeotropic distillation with CHCl3 3 times. The resultant was basified with aqueous 2N potassium hydroxide solution (20 ml) and extracted with CHCl3 3 times. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, filtered and distilled under reduced pressure to obtain 433 mg of the title compound as yellow oil (yield 86%). The resulting mixture was reacted for 18 hrs After the completion of reaction the reaction mixture was distilled concentrated under reduced pressure subjected to azeotropic distillation with CHCl3 3 times extracted with CHCl3 3 times The organic layer was separated washed with brine dried over anhydrous magnesium sulfate filtered distilled under reduced pressure