ethyl 3,3-dimethyl-2-oxobutanoate

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

実験手順: The procedure described under h) was carried out using 15 g of ethyl trimethyl-pyruvate and 50 g of (R)-1-phenylethylamine. There were isolated 14.9 g of (47%) of (R)-3,3-dimethyl-N-[(R)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 95°-96° C. [α]=+59.6 (c=1.0, CHCl3).

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

実験手順: A solution of 15 g (95 mmol) of ethyl trimethyl-pyruvate and 50 g (413 mmol) of (S)-1-phenylethylamine in 50 ml of xylene was boiled under reflux on a water separator for 18 hours. Subsequently, the solvent was distilled off and excess amine was removed at 120° C. in a vacuum. After crystallization of the distillation residue from 125 ml of hexane there were obtained 14.3 g (45%) of (S)-3,3-dimethyl-N-[(S)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 96°-97° C. [α]=-58.9 (c=1.0, CHCl3). Subsequently, the solvent was distilled off excess amine was removed at 120° C. in a vacuum After crystallization of the distillation residue from 125 ml of hexane

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

実験手順: A solution of 15 g (95 mmol) of ethyl trimethyl-pyruvate and 50 g (413 mmol) of (S)-1-phenylethylamine in 50 ml of xylene was boiled under reflux on a water separator for 18 hours. Subsequently, the solvent was distilled off and excess amine was removed at 120° C. in a vacuum. After crystallization of the distillation residue from 125 ml of hexane there were obtained 14.3 g (45%) of (S)-3,3-dimethyl-N-[(S)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 96°-97° C. [α]=-58.9 (c=1.0, CHCl3). Subsequently, the solvent was distilled off excess amine was removed at 120° C. in a vacuum After crystallization of the distillation residue from 125 ml of hexane

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

実験手順: The procedure described under h) was carried out using 15 g of ethyl trimethyl-pyruvate and 50 g of (R)-1-phenylethylamine. There were isolated 14.9 g of (47%) of (R)-3,3-dimethyl-N-[(R)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 95°-96° C. [α]=+59.6 (c=1.0, CHCl3).

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

実験手順: A solution of 15 g (95 mmol) of ethyl trimethyl-pyruvate and 50 g (413 mmol) of (S)-1-phenylethylamine in 50 ml of xylene was boiled under reflux on a water separator for 18 hours. Subsequently, the solvent was distilled off and excess amine was removed at 120° C. in a vacuum. After crystallization of the distillation residue from 125 ml of hexane there were obtained 14.3 g (45%) of (S)-3,3-dimethyl-N-[(S)-1-phenylethyl]-2-(1-phenylethylimino)-butyramide of melting point 96°-97° C. [α]=-58.9 (c=1.0, CHCl3). Subsequently, the solvent was distilled off excess amine was removed at 120° C. in a vacuum After crystallization of the distillation residue from 125 ml of hexane