3-bromopiperidin-2-one

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2.0 g of 3-bromopiperidin-2-one in 30 ml of N,N-dimethylformamide was added 5.9 g of sodium azide, followed by stirring at 60° C. overnight. After cooling down to room temperature, water was added to the reaction mixture and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 890 mg of the title compound as a yellow oil. After cooling down to room temperature the mixture was extracted with ethyl acetate The organic layer was washed with water and saturated brine dried over anhydrous magnesium sulfate the solvent was evaporated

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2.0 g of 3-bromopiperidin-2-one in 30 ml of N,N-dimethylformamide was added 5.9 g of sodium azide, followed by stirring at 60° C. overnight. After cooling down to room temperature, water was added to the reaction mixture and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 890 mg of the title compound as a yellow oil. After cooling down to room temperature the mixture was extracted with ethyl acetate The organic layer was washed with water and saturated brine dried over anhydrous magnesium sulfate the solvent was evaporated

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 2.0 g of 3-bromopiperidin-2-one in 30 ml of N,N-dimethylformamide was added 5.9 g of sodium azide, followed by stirring at 60° C. overnight. After cooling down to room temperature, water was added to the reaction mixture and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 890 mg of the title compound as a yellow oil. After cooling down to room temperature the mixture was extracted with ethyl acetate The organic layer was washed with water and saturated brine dried over anhydrous magnesium sulfate the solvent was evaporated

反応条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 3-Bromopiperidin-2-one 51-1 (0.15 g, 0.87 mmol) was dissolved in n-butanol (4 mL) then triethyl amine (0.26 g, 2.60 mmol) was added followed by tert-butyl piperazine-1-carboxylate 12-1 (0.16 g, 0.87 mmol). This was then stirred at 150° C. for 1.5 hours and then the solid was filtered off, washed with n-butanol and then ethyl ether. Hi-Res MS: calc: 284.1969 found: 284.1966. 1H-NMR (CDCl3): 3.45 (br s, 2H); 3.26 (br s, 2H); 3.13 (complex, 3H); 2.74(m, 1H); 2.62(m, 1H); 1.98(m, 1H); 1.77(m, 1H); 1.55(complex, 3H); 1.45(t, 9H). the solid was filtered off washed with n-butanol

反応条件: temp:0.00; pressure:0.00; stir: