脱氧麻黄碱

反应条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 4,6-dichloro-2-pyrimidinamine (1.0 g, 6.10 mmol) and K2CO3 (1.69 g, 12.2 mmol) in CH3CN (6.0 mL) was added (2R)—N-methyl-1-phenyl-2-propanamine (1.09 g, 7.32 mmol), and the reaction mixture was heated at 140° C. under microwave conditions with stirring for 2 hours. The mixture was filtered and washed by EtOAc (50 mL). The solution was concentrated, and the resulting residue was purified by reversed phase chromatography using CH3CN in water from 45% to 55% (0.5% ammonium hydrogen carbonate in water) to afford the title compound (910 mg) as a white solid. LC-MS (ES) m/z=277 [M+H]+. The mixture was filtered washed by EtOAc (50 mL) The solution was concentrated the resulting residue was purified by reversed phase chromatography

反应条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 4,6-dichloro-2-pyrimidinamine (1.0 g, 6.10 mmol) and K2CO3 (1.69 g, 12.2 mmol) in CH3CN (6.0 mL) was added (2R)—N-methyl-1-phenyl-2-propanamine (1.09 g, 7.32 mmol), and the reaction mixture was heated at 140° C. under microwave conditions with stirring for 2 hours. The mixture was filtered and washed by EtOAc (50 mL). The solution was concentrated, and the resulting residue was purified by reversed phase chromatography using CH3CN in water from 45% to 55% (0.5% ammonium hydrogen carbonate in water) to afford the title compound (910 mg) as a white solid. LC-MS (ES) m/z=277 [M+H]+. The mixture was filtered washed by EtOAc (50 mL) The solution was concentrated the resulting residue was purified by reversed phase chromatography

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred suspension LiAlH4 (0.77 g, 20.4 mmol) in THF (120 mL) was added a solution of 1,1-dimethylethyl[(1R)-1-methyl-2-phenylethyl]carbamate (2.4 g, 10.2 mmol) in THF (30.0 ml) dropwise at 0° C., and then the reaction mixture was heated at reflux for 2 hours. The mixture was cooled to 0° C., and quenched by addition of ice (1.0 g), then 15% aqueous sodium hydroxide (1.0 mL) followed by water (0.5 mL). The lithium salts were collected by filtration and washed with Et2O (200 mL). The filtrate was dried (Na2SO4), filtered and concentrated. The resulting residue was distilled at reduced pressure to afford the title compound (1.6 g) as a light yellow oil. LC-MS (ES) m/z=150 [M+H]+. the reaction mixture was heated at reflux for 2 hours quenched by addition of ice (1.0 g) The lithium salts were collected by filtration washed with Et2O (200 mL) The filtrate was dried (Na2SO4) filtered concentrated The resulting residue was distilled at reduced pressure