N-[(4-苄基吗啉-2-基)甲基]乙酰胺

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:; See reaction.notes.procedure_details.

实验步骤: 2-Acetylaminomethyl-4-benzylmorpholine (120 g) is dissolved in a mixture of ethanol (1000 ml) and acetic acid (30 ml) and hydrogenated over 10% palladium on carbon (5 g) at about 60° C. After the calculated amount of the hydrogen is absorbed, the catalyst is filtered off. The filtrate is evaporated under reduced pressure to give the title compound as an oil. After the calculated amount of the hydrogen is absorbed the catalyst is filtered off The filtrate is evaporated under reduced pressure

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

实验步骤: A mixture of N-[(4-benzyl-2-morpholinyl)methyl]phthalimide (162 g), 85% hydrazine hydrate (43.3 g), and ethanol (100 ml) is refluxed with stirring for 20 minutes. The reaction mixture is filtered, and the filtrate is diluted with water and extracted with chloroform. The organic layer is separated, washed with a small amount of water and then with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and filtered. To the filtrate is added slowly acetic anhydride (98.3 g), and the resulting mixture is stirred at 25° C. for 2 hours. The reaction mixture is washed successively with aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is recrystallized from toluene to give the title compound (101 g), mp 110°-111° C. is refluxed The reaction mixture is filtered the filtrate is diluted with water extracted with chloroform The organic layer is separated washed with a small amount of water with saturated aqueous sodium chloride solution, dried over magnesium sulfate filtered To the filtrate is added slowly acetic anhydride (98.3 g) the resulting mixture is stirred at 25° C. for 2 hours The reaction mixture is washed successively with aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution dried over magnesium sulfate The solvent is distilled off under reduced pressure the residue is recrystallized from toluene

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a solution of 2-(N-acetylaminomethyl)-4-benzylmorpholine (20 g, 80.7 mmol) in ethanol-acetic acid (20/1, 210 ml) was suspended 2.0 g of 10% palladium-carbon and the mixture was stirred at 60° C. under hydrogen stream for 22 hours. The reaction mixture was filtered with Celite, the solvent was distilled off from the filtrate under reduced pressure to give crude 2-(N-acetylaminomethyl)morpholine (15.62 g). Yield=100%. This compound was used for the subsequent reaction without purification. The reaction mixture was filtered with Celite the solvent was distilled off from the filtrate under reduced pressure

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

实验步骤: To a solution of crude 2-aminomethyl-4-benzylmorpholine (48 g) in toluene (400 ml) was added pyridine (24.5 ml, 0.303 mol) and then acetic anhydride (26.4 ml, 0.280 mol) was added dropwise under ice-cooling over 10 minutes and then allowed to rise to room temperature and the mixture was stirred for one hour. To the reaction mixture was added aqueous saturated sodium hydrogen carbonate (200 ml) under ice-cooling and then 10% aqueous sodium hydroxide was added until the mixture became strongly basic. The reaction mixture was extracted with ethyl acetate (200 ml×3) and the combined organic layer was washed with aqueous saturated sodium chloride (200 ml). The organic layer was dried over potassium carbonate and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate-hexane (1/1) to give 2-(N-acetylaminomethyl)-4-benzylmorpholine (25.93 g). A total yield of 3 steps=56%. cooling over 10 minutes to rise to room temperature cooling The reaction mixture was extracted with ethyl acetate (200 ml×3) the combined organic layer was washed with aqueous saturated sodium chloride (200 ml) The organic layer was dried over potassium carbonate the solvent was distilled off under reduced pressure The residue was recrystallized from ethyl acetate-hexane (1/1)