卡西酮

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Oxalyl chloride (1.17 mL, 13.3 mmol) was added to the suspension of 4-(phenylmethyl)-2-morpholinecarboxylic acid (2.290 g, 8.89 mmol) and DMF (0.034 mL, 0.444 mmol) in CH2Cl2 (60 mL) at 0° C., and the resulting mixture was stirred at 25° C. for 2 hours, and then evaporated. CH2Cl2 (60 mL) was added to the resulting residue, and the resulting brown solution was added to a suspension of triethylamine (4.34 mL, 31.1 mmol) and 2-amino-1-phenyl-1-propanone (1.65 g, 8.89 mmol) in CH2Cl2 (60 mL) at 0° C. The reaction mixture was stirred at 25° C. overnight. Water (150 mL) was added, and the resulting mixture was extracted with EtOAc (3×80 mL). The organics were dried (Na2SO4), filtered, and evaporated. The resulting residue was purified by silica gel chromatography, eluting with EtOAc in PE from 20% to 50% to afford the title compound (1.3 g) as a yellow oil. LC-MS (ES) m/z=353 [M+H]+. evaporated CH2Cl2 (60 mL) was added to the resulting residue The reaction mixture was stirred at 25° C. overnight the resulting mixture was extracted with EtOAc (3×80 mL) The organics were dried (Na2SO4) filtered evaporated The resulting residue was purified by silica gel chromatography eluting with EtOAc in PE from 20% to 50%

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Oxalyl chloride (1.17 mL, 13.3 mmol) was added to the suspension of 4-(phenylmethyl)-2-morpholinecarboxylic acid (2.290 g, 8.89 mmol) and DMF (0.034 mL, 0.444 mmol) in CH2Cl2 (60 mL) at 0° C., and the resulting mixture was stirred at 25° C. for 2 hours, and then evaporated. CH2Cl2 (60 mL) was added to the resulting residue, and the resulting brown solution was added to a suspension of triethylamine (4.34 mL, 31.1 mmol) and 2-amino-1-phenyl-1-propanone (1.65 g, 8.89 mmol) in CH2Cl2 (60 mL) at 0° C. The reaction mixture was stirred at 25° C. overnight. Water (150 mL) was added, and the resulting mixture was extracted with EtOAc (3×80 mL). The organics were dried (Na2SO4), filtered, and evaporated. The resulting residue was purified by silica gel chromatography, eluting with EtOAc in PE from 20% to 50% to afford the title compound (1.3 g) as a yellow oil. LC-MS (ES) m/z=353 [M+H]+. evaporated CH2Cl2 (60 mL) was added to the resulting residue The reaction mixture was stirred at 25° C. overnight the resulting mixture was extracted with EtOAc (3×80 mL) The organics were dried (Na2SO4) filtered evaporated The resulting residue was purified by silica gel chromatography eluting with EtOAc in PE from 20% to 50%

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Palladium on carbon (1.069 g, 1.005 mmol) was added to the solution of 2-azido-1-phenyl-1-propanone (1.76 g, 10.05 mmol) and hydrochloric acid (6.69 mL, 80 mmol) in CH3OH (50 mL) under nitrogen, and the reaction mixture was stirred under hydrogen overnight at 25° C. The mixture was filtered, washing with CH2Cl2 (50 mL) and CH3OH (100 mL), and concentrated. Water (100 mL) was added, and the resulting mixture was lyophilized to yield an HCl salt of the title compound (1.9 g) as a brown solid. LC-MS (ES) m/z=150 [M+H]+. The mixture was filtered washing with CH2Cl2 (50 mL) and CH3OH (100 mL) concentrated Water (100 mL) was added