CHEMBRDG-BB 4014220

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: To the imine from isobutyraldehyde and benzylamine (48.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole) and the mixture slowly warmed while stirring. As the internal temperature reached 70°-75° a vigorous exothermic reaction ensued taking the temperature to 130°-135°. After maintaining at 130°-140° for 30 mins. the viscous product was cooled to 100° and diluted with water. Basification and extraction with chloroform gave crude amine after solvent evaporation. Distillation gave pure N-benzylisobutylamine, 13.6 g (28%) bp 94°-99°/5.6 mm. Nmr confirmed the assigned structure. the mixture slowly warmed reached 70°-75° a vigorous exothermic reaction to 130°-135° After maintaining at 130°-140° for 30 mins the viscous product was cooled to 100° Basification and extraction with chloroform gave crude amine after solvent evaporation Distillation

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

实验步骤: To a stirred solution of lithium aluminum hydride (23 g, 606 mmol) in ether (115 ml) was added an ethereal solution (115 ml) of N-benzylidene-2-methyl-1-propanamine (72.1 g, 447 mmol) over a period of 45 minutes. It was then refluxed for one hour. The reaction mixture was cooled in an ice bath and while stirring vigorously, aqueous sodium hydroxide (20%, 120 ml) was added dropwise. The ether solution was separated, dried over magnesium sulfate and concentrated to dryness yielding 66.1 g of the title compound. It was then refluxed for one hour The reaction mixture was cooled in an ice bath The ether solution was separated dried over magnesium sulfate concentrated to dryness

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

实验步骤: To a stirred solution of lithium aluminum hydride (23 g, 606 mmol) in ether (115 ml) was added an ethereal solution (115 ml) of N-benzylidene-2-methyl-1-propanamine (72.1 g, 447 mmol) over a period of 45 minutes. It was then refluxed for one hour. The reaction mixture was cooled in an ice bath and while stirring vigorously, aqueous sodium hydroxide (20%, 120 ml) was added dropwise. The ether solution was separated, dried over magnesium sulfate and concentrated to dryness yielding 66.1 g of the title compound. It was then refluxed for one hour The reaction mixture was cooled in an ice bath The ether solution was separated dried over magnesium sulfate concentrated to dryness

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

实验步骤: To the imine from isobutyraldehyde and benzylamine (48.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole) and the mixture slowly warmed while stirring. As the internal temperature reached 70°-75° a vigorous exothermic reaction ensued taking the temperature to 130°-135°. After maintaining at 130°-140° for 30 mins. the viscous product was cooled to 100° and diluted with water. Basification and extraction with chloroform gave crude amine after solvent evaporation. Distillation gave pure N-benzylisobutylamine, 13.6 g (28%) bp 94°-99°/5.6 mm. Nmr confirmed the assigned structure. the mixture slowly warmed reached 70°-75° a vigorous exothermic reaction to 130°-135° After maintaining at 130°-140° for 30 mins the viscous product was cooled to 100° Basification and extraction with chloroform gave crude amine after solvent evaporation Distillation

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

实验步骤: To the imine from isobutyraldehyde and benzylamine (48.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole) and the mixture slowly warmed while stirring. As the internal temperature reached 70°-75° a vigorous exothermic reaction ensued taking the temperature to 130°-135°. After maintaining at 130°-140° for 30 mins. the viscous product was cooled to 100° and diluted with water. Basification and extraction with chloroform gave crude amine after solvent evaporation. Distillation gave pure N-benzylisobutylamine, 13.6 g (28%) bp 94°-99°/5.6 mm. Nmr confirmed the assigned structure. the mixture slowly warmed reached 70°-75° a vigorous exothermic reaction to 130°-135° After maintaining at 130°-140° for 30 mins the viscous product was cooled to 100° Basification and extraction with chloroform gave crude amine after solvent evaporation Distillation

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

实验步骤: To the imine from isobutyraldehyde and benzylamine (51.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole). While stirring the mixture was slowly warmed to 65°-70° when a vigorous exothermic reaction was initiated. The reaction temperature reached 130°-145°. Upon cooling the reaction mixture became a glass. This glass was dissolved in water and basified. Extraction with benzene yielded benzylisobutylamine. The aqueous portion was acidified and after removal of sodium chloride yielded a phosphonic acid (20 g). Recrystallization gave a white solid (12 g) mp 186°-190° the N-benzyl α-aminophosphonic acid. ##STR35## was slowly warmed to 65°-70° when a vigorous exothermic reaction reached 130°-145° Upon cooling the reaction mixture Extraction with benzene

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

实验步骤: To the imine from isobutyraldehyde and benzylamine (51.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole). While stirring the mixture was slowly warmed to 65°-70° when a vigorous exothermic reaction was initiated. The reaction temperature reached 130°-145°. Upon cooling the reaction mixture became a glass. This glass was dissolved in water and basified. Extraction with benzene yielded benzylisobutylamine. The aqueous portion was acidified and after removal of sodium chloride yielded a phosphonic acid (20 g). Recrystallization gave a white solid (12 g) mp 186°-190° the N-benzyl α-aminophosphonic acid. ##STR35## was slowly warmed to 65°-70° when a vigorous exothermic reaction reached 130°-145° Upon cooling the reaction mixture Extraction with benzene

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: To a stirred solution of lithium aluminum hydride (23 g, 606 mmol) in ether (115 ml) was added an ethereal solution (115 ml) of N-benzylidene-2-methyl-1-propanamine (72.1 g, 447 mmol) over a period of 45 minutes. It was then refluxed for one hour. The reaction mixture was cooled in an ice bath and while stirring vigorously, aqueous sodium hydroxide (20%, 120 ml) was added dropwise. The ether solution was separated, dried over magnesium sulfate and concentrated to dryness yielding 66.1 g of the title compound. It was then refluxed for one hour The reaction mixture was cooled in an ice bath The ether solution was separated dried over magnesium sulfate concentrated to dryness

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

实验步骤: To the imine from isobutyraldehyde and benzylamine (48.4 g; 0.3 mole) was added phosphorous acid (24.6 g; 0.3 mole) and the mixture slowly warmed while stirring. As the internal temperature reached 70°-75° a vigorous exothermic reaction ensued taking the temperature to 130°-135°. After maintaining at 130°-140° for 30 mins. the viscous product was cooled to 100° and diluted with water. Basification and extraction with chloroform gave crude amine after solvent evaporation. Distillation gave pure N-benzylisobutylamine, 13.6 g (28%) bp 94°-99°/5.6 mm. Nmr confirmed the assigned structure. the mixture slowly warmed reached 70°-75° a vigorous exothermic reaction to 130°-135° After maintaining at 130°-140° for 30 mins the viscous product was cooled to 100° Basification and extraction with chloroform gave crude amine after solvent evaporation Distillation