N-tert-butyl-N',N'-dimethylethane-1,2-diamine

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

実験手順: Into a 50 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 16 g (0.22 mol) of t-butylamine, 5.0 g (35 mmol) of 2-(dimethylamino)ethyl chloride hydrochloride and 1 ml of water. And then, the mixture was reacted at 70° C. for 10 hours. After the completion of the reaction, the reaction solution was subjected to extraction with 25 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa), to provide 3.0 g of 1-(t-butylamino)-2-dimethylaminoethane. (Isolation yield: 60%) Into a 50 mL-volume flask equipped with a stirrer And then, the mixture was reacted at 70° C. for 10 hours After the completion of the reaction the reaction solution was subjected to extraction with 25 ml of hexane twice the hexane layer was concentrated under reduced pressure The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa)

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

実験手順: Into a 50 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 16 g (0.22 mol) of t-butylamine, 5.0 g (35 mmol) of 2-(dimethylamino)ethyl chloride hydrochloride and 1 ml of water. And then, the mixture was reacted at 70° C. for 10 hours. After the completion of the reaction, the reaction solution was subjected to extraction with 25 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa), to provide 3.0 g of 1-(t-butylamino)-2-dimethylaminoethane. (Isolation yield: 60%) Into a 50 mL-volume flask equipped with a stirrer And then, the mixture was reacted at 70° C. for 10 hours After the completion of the reaction the reaction solution was subjected to extraction with 25 ml of hexane twice the hexane layer was concentrated under reduced pressure The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa)

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-(t-Butylamino)ethylchloride hydrochloride (1.2 g, 7.0 mmol) is dissolved in aqueous dimethylamine solution (40% by weight, 22 mL) in a sealed tube. The mixture is heated in a 140° C. oil bath for six hours, allowed to cool to room temperature, and then is saturated with solid potassium carbonate. The mixture is extracted thrice with ethyl acetate. The combined extracts are dried over anhydrous sodium sulfate, decanted, and concentrated under reduced pressure to give N-t-butyl,N′,N′-dimethylethylenediamine as a light brown liquid (0.57 g, 56%). The crude material is carried on to the following step without further purification. to cool to room temperature The mixture is extracted thrice with ethyl acetate The combined extracts are dried over anhydrous sodium sulfate decanted concentrated under reduced pressure

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

実験手順: Into a 50 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 16 g (0.22 mol) of t-butylamine, 5.0 g (35 mmol) of 2-(dimethylamino)ethyl chloride hydrochloride and 1 ml of water. And then, the mixture was reacted at 70° C. for 10 hours. After the completion of the reaction, the reaction solution was subjected to extraction with 25 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa), to provide 3.0 g of 1-(t-butylamino)-2-dimethylaminoethane. (Isolation yield: 60%) Into a 50 mL-volume flask equipped with a stirrer And then, the mixture was reacted at 70° C. for 10 hours After the completion of the reaction the reaction solution was subjected to extraction with 25 ml of hexane twice the hexane layer was concentrated under reduced pressure The resultant concentrate was distilled under reduced pressure (60° C., 2.4 kPa)