反应详情

A solution of 35.0 g (271 mmol) of 3,3-dimethyl-2-oxobutyramide and 75.0 g (619 mmol) of (S)-1-phenylethylamine in 250 ml of toluene was boiled under reflux on a water separator for 92 hours. Subsequently, the solvent and excess amine were removed in a vacuum. The residual oil was crystallized from 300 ml of hexane. 51 g of crude material of melting point 96°-97° C. were obtained. After recrystallization from 400 ml of hexane there were obtained 42.7 g (68%) of analytically-pure (S)-3,3-dimethyl-2-(1-phenylethylimino)-butyramide of melting point 100°-101° C. [α]=-58.5 (c=1.0, CHCl3).

1. customSubsequently, the solvent and excess amine were removed in a vacuum
2. customThe residual oil was crystallized from 300 ml of hexane
3. custom51 g of crude material of melting point 96°-97° C. were obtained
4. customAfter recrystallization from 400 ml of hexane