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Ethyl Acetate → ethyl (2R, 3S)-3-methoxy-2-methylbutyrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | ethyl-(2R)-methyl-(3S)-hydroxybutanoate | HCID 642623 | — |
| 反応物 | Methyl iodate | HCID 13203471 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | ethyl (2R, 3S)-3-methoxy-2-methylbutyrate | HCID 57158131 | 76.4% |
反応手順
Ethyl (2R, 3S)-3-hydroxy-2-methylbutyrate (8.20 g) and methyl iodate (78.0 g) were dissolved in N,N-dimethylformamide (150 ml). To this solution was added sodium hydride (about 60% in oil, 2.46 g) little by little with ice cooling and the mixture was stirred for 1 hour with ice cooling. The reaction mixture was poured into ethyl acetate (300 ml) and the mixture was stirred for 10 minutes. Insoluble materials were filtered off and the filtrate was washed 3 times with water. The organic layer was dried, concentrated and distilled under reduced pressure (b.p. 80° C./30 mmHg) to obtain ethyl (2R, 3S)-3-methoxy-2-methylbutyrate (6.87 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05232853 |
| 出典データセット | uspto-grants-1993_08 |
| ORD ID | ord-e9b8d2372f61430f882f6799184a0467 |
| 出典メモ | uspto-grants-1993_08 |