4-(二乙基氨基)丁酸

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: N,N'-Carbonyldiimidazole (11.2 g) was added to a suspension of 4-(N,N-diethylamino)butanoic acid (10.0 g) in tetrahydrofuran (400 ml), and the mixture was stirred at room temperature for 6 hours. Then monoethyl malonate magnesium salt (Mg(OCOCH2COOC2H5)2)(19.8 g) was added, and the mixture was stirred at room temperature for 14 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-methanol (5:1, v/v) gave ethyl 6-(N,N-diethylamino)-3-oxohexanoate (7.6 g, 53%). the mixture was stirred at room temperature for 14 hours The reaction mixture was concentrated under reduced pressure the residue was dissolved in chloroform The chloroform layer was washed with water dried over magnesium sulfate the solvent was evaporated under reduced pressure The fractions eluted with chloroform-methanol (5:1

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

实验步骤: N,N'-Carbonyldiimidazole (11.2 g) was added to a suspension of 4-(N,N-diethylamino)butanoic acid (10.0 g) in tetrahydrofuran (400 ml), and the mixture was stirred at room temperature for 6 hours. Then monoethyl malonate magnesium salt (Mg(OCOCH2COOC2H5)2)(19.8 g) was added, and the mixture was stirred at room temperature for 14 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-methanol (5:1, v/v) gave ethyl 6-(N,N-diethylamino)-3-oxohexanoate (7.6 g, 53%). the mixture was stirred at room temperature for 14 hours The reaction mixture was concentrated under reduced pressure the residue was dissolved in chloroform The chloroform layer was washed with water dried over magnesium sulfate the solvent was evaporated under reduced pressure The fractions eluted with chloroform-methanol (5:1

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

实验步骤: A mixture of benzyl 4-(N,N-diethylamino)butanoate (33.8 g), palladium-carbon (5%, 7 g) and ethanol (500 ml) was subjected to catalytic hydrogenation at room temperature and 1 atm. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give 4-(N,N-diethylamino)butanoic acid (16.2 g, 75%). mp. 45°-47° C. was subjected to catalytic hydrogenation at room temperature The catalyst was filtered off the filtrate was concentrated 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 benzyl 4-(N,N-diethylamino)butanoate (33.8 g), palladium-carbon (5%, 7 g) and ethanol (500 ml) was subjected to catalytic hydrogenation at room temperature and 1 atm. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give 4-(N,N-diethylamino)butanoic acid (16.2 g, 75%). mp. 45°-47° C. was subjected to catalytic hydrogenation at room temperature The catalyst was filtered off the filtrate was concentrated under reduced pressure

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

实验步骤: N,N'-Carbonyldiimidazole (11.2 g) was added to a suspension of 4-(N,N-diethylamino)butanoic acid (10.0 g) in tetrahydrofuran (400 ml), and the mixture was stirred at room temperature for 6 hours. Then monoethyl malonate magnesium salt (Mg(OCOCH2COOC2H5)2)(19.8 g) was added, and the mixture was stirred at room temperature for 14 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-methanol (5:1, v/v) gave ethyl 6-(N,N-diethylamino)-3-oxohexanoate (7.6 g, 53%). the mixture was stirred at room temperature for 14 hours The reaction mixture was concentrated under reduced pressure the residue was dissolved in chloroform The chloroform layer was washed with water dried over magnesium sulfate the solvent was evaporated under reduced pressure The fractions eluted with chloroform-methanol (5:1

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

实验步骤: A mixture of benzyl 4-(N,N-diethylamino)butanoate (33.8 g), palladium-carbon (5%, 7 g) and ethanol (500 ml) was subjected to catalytic hydrogenation at room temperature and 1 atm. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give 4-(N,N-diethylamino)butanoic acid (16.2 g, 75%). mp. 45°-47° C. was subjected to catalytic hydrogenation at room temperature The catalyst was filtered off the filtrate was concentrated under reduced pressure

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: N,N'-Carbonyldiimidazole (11.2 g) was added to a suspension of 4-(N,N-diethylamino)butanoic acid (10.0 g) in tetrahydrofuran (400 ml), and the mixture was stirred at room temperature for 6 hours. Then monoethyl malonate magnesium salt (Mg(OCOCH2COOC2H5)2)(19.8 g) was added, and the mixture was stirred at room temperature for 14 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried over magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was subjected to column chromatography on silica gel. The fractions eluted with chloroform-methanol (5:1, v/v) gave ethyl 6-(N,N-diethylamino)-3-oxohexanoate (7.6 g, 53%). the mixture was stirred at room temperature for 14 hours The reaction mixture was concentrated under reduced pressure the residue was dissolved in chloroform The chloroform layer was washed with water dried over magnesium sulfate the solvent was evaporated under reduced pressure The fractions eluted with chloroform-methanol (5:1

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

实验步骤: A mixture of benzyl 4-(N,N-diethylamino)butanoate (33.8 g), palladium-carbon (5%, 7 g) and ethanol (500 ml) was subjected to catalytic hydrogenation at room temperature and 1 atm. The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give 4-(N,N-diethylamino)butanoic acid (16.2 g, 75%). mp. 45°-47° C. was subjected to catalytic hydrogenation at room temperature The catalyst was filtered off the filtrate was concentrated under reduced pressure