tert-butyl 2-(cyclopropylamino)acetate

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To a solution of N-(cyclopropyl)glycine t-butyl ester (12 g, 0.0702 mol) and 3-acetylthio-2-methylpropionic acid (8.1 g, 0.050 mol) in methylene chloride (200 ml) chilled in an ice bath was added dicyclohexylcarbodiimide (14.4 g, 0.070 mol). The resulting mixture was stirred for sixteen hours at room temperature. The dicyclohexylurea was removed by filtration and washed with diethyl ether. Evaporation of the filtrate yielded the crude product as a pale yellow oil which was used without further purification. The dicyclohexylurea was removed by filtration washed with diethyl ether Evaporation of the filtrate

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

実験手順: Cyclopropylamine (19.5 g, 0.342 mol) was placed in a pressure bottle and ethanol (100 ml.) was added. The resulting solution was cooled in an ice bath and sodium bicarbonate (8.5 g, 0.101 mol) and t-butyl bromoacetate (15.5 g, 0.0795 mol) was added. The flask was stoppered and the contents of the flask were stirred for 30 minutes with external cooling (ice bath) and then at room temperature overnight. Most of the solvent was removed on a rotary evaporator and water was added to the residue. The product was extracted several times with chloroform. The combined chloroform extract was washed with water, dried over sodium sulfate, filtered and evaporated to yield the product as a pale yellow oil (12.5 g, 92%). was added The resulting solution was cooled in an ice bath with external cooling (ice bath) at room temperature overnight Most of the solvent was removed on a rotary evaporator and water was added to the residue The product was extracted several times with chloroform The combined chloroform extract was washed with water dried over sodium sulfate filtered evaporated

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: To a solution of N-(cyclopropyl)glycine t-butyl ester (12 g, 0.0702 mol) and 3-acetylthio-2-methylpropionic acid (8.1 g, 0.050 mol) in methylene chloride (200 ml) chilled in an ice bath was added dicyclohexylcarbodiimide (14.4 g, 0.070 mol). The resulting mixture was stirred for sixteen hours at room temperature. The dicyclohexylurea was removed by filtration and washed with diethyl ether. Evaporation of the filtrate yielded the crude product as a pale yellow oil which was used without further purification. The dicyclohexylurea was removed by filtration washed with diethyl ether Evaporation of the filtrate

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

実験手順: Cyclopropylamine (19.5 g, 0.342 mol) was placed in a pressure bottle and ethanol (100 ml.) was added. The resulting solution was cooled in an ice bath and sodium bicarbonate (8.5 g, 0.101 mol) and t-butyl bromoacetate (15.5 g, 0.0795 mol) was added. The flask was stoppered and the contents of the flask were stirred for 30 minutes with external cooling (ice bath) and then at room temperature overnight. Most of the solvent was removed on a rotary evaporator and water was added to the residue. The product was extracted several times with chloroform. The combined chloroform extract was washed with water, dried over sodium sulfate, filtered and evaporated to yield the product as a pale yellow oil (12.5 g, 92%). was added The resulting solution was cooled in an ice bath with external cooling (ice bath) at room temperature overnight Most of the solvent was removed on a rotary evaporator and water was added to the residue The product was extracted several times with chloroform The combined chloroform extract was washed with water dried over sodium sulfate filtered evaporated

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

実験手順: To a solution of N-(cyclopropyl)glycine t-butyl ester (12 g, 0.0702 mol) and 3-acetylthio-2-methylpropionic acid (8.1 g, 0.050 mol) in methylene chloride (200 ml) chilled in an ice bath was added dicyclohexylcarbodiimide (14.4 g, 0.070 mol). The resulting mixture was stirred for sixteen hours at room temperature. The dicyclohexylurea was removed by filtration and washed with diethyl ether. Evaporation of the filtrate yielded the crude product as a pale yellow oil which was used without further purification. The dicyclohexylurea was removed by filtration washed with diethyl ether Evaporation of the filtrate

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

実験手順: Cyclopropylamine (19.5 g, 0.342 mol) was placed in a pressure bottle and ethanol (100 ml.) was added. The resulting solution was cooled in an ice bath and sodium bicarbonate (8.5 g, 0.101 mol) and t-butyl bromoacetate (15.5 g, 0.0795 mol) was added. The flask was stoppered and the contents of the flask were stirred for 30 minutes with external cooling (ice bath) and then at room temperature overnight. Most of the solvent was removed on a rotary evaporator and water was added to the residue. The product was extracted several times with chloroform. The combined chloroform extract was washed with water, dried over sodium sulfate, filtered and evaporated to yield the product as a pale yellow oil (12.5 g, 92%). was added The resulting solution was cooled in an ice bath with external cooling (ice bath) at room temperature overnight Most of the solvent was removed on a rotary evaporator and water was added to the residue The product was extracted several times with chloroform The combined chloroform extract was washed with water dried over sodium sulfate filtered evaporated