関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methyl 2-((benzoylamino)methyl)-3-oxobutanoate | HCID 11831808 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | methyl (2R, 3S)-2-(N-benzoylamino)methyl-3-hydroxybutanoate | HCID 10264162 | 91% |
反応手順
In a 100 ml-volume autoclave whose atmosphere had been displaced with nitrogen was added a methylene chloride solution of 2.5 g of methyl 2-(N-benzoylamino)methyl-3-oxobutanoate and 84.5 mg (0.05 mmole) of Ru2Cl4 ((-)-BINAP2 (NEt3), and a reaction was conducted by stirring at 45° C. under a hydrogen pressure of 70 kg/cm2 for 24 hours. The reaction mixture was taken out, and the solvent was removed by distillation under reduced pressure of 20 mmHg at 30° C. The residue was purified by silica gel column chromatography using a 7/3 (by volume) mixture of hexane and isopropanol as an eluent to obtain 2.27 g (yield: 91%) of methyl (2R, 3S)-2-(N-benzoylamino)methyl-3-hydroxybutanoate having an optical purity of 97 %ee.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04981992 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-40ea430dc7dc49dbb7f8848a2d950e32 |
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| 出典メモ | uspto-grants-1991_01 |
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