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Water → (S)-N-tert-butyl-3,3-dimethyl-2-(1-phenylethylimino)-butyramide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Phenethylamine, (-)- | HCID 75818 | — |
| 反応物 | N-tert-Butyl-3,3-dimethyl-2-oxobutanamide | HCID 13355144 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (S)-N-tert-butyl-3,3-dimethyl-2-(1-phenylethylimino)-butyramide | HCID 54448077 | 80% |
反応手順
A solution of 30.0 g (162 mmol) of N-tert-butyl-3,3-dimethyl-2-oxo-butyramide (D. Seyferth, R. C. Hui, Tetrahedron Lett. 1984, 25, 5251) and 50 g (413 mmol) of (S)-1-phenylethylamine in 150 ml of toluene was boiled under reflux on a water separator for 20 hours. Subsequently, the solvent and excess amine were removed in a vacuum. The residue was treated with 200 ml of hexane at 0° C. and stirred. After filtration of the suspension and concentration in a vacuum the residual oil was distilled. There were obtained 37.2 g (80%) of (S)-N-tert-butyl-3,3-dimethyl-2-(1-phenylethylimino)-butyramide of boiling point 140° C. at 0.3 mbar. [α]=-40.7 (c=1.0, CHCl3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05710322 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-239b7e6c7b324a818673d6f0498f1758 |
| 出典メモ | uspto-grants-1998_01 |