関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Formate | HCID 2735122 | — |
| 反応物 | N-benzyl-4-bromo-3-oxobutanamide | HCID 71502812 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-benzyl-4-hydroxy-3-oxobutanamide | HCID 71502813 | 54.6% |
反応手順
N-benzyl-4-bromo-3-oxobutanamide (compound B 50 g, 185.1 mmol) was dissolved in methanol (400 ml), and potassium formate (31.14 g, 370.2 mmol) was added. The resulting mixture was heated under reflux for 2 hours. Methanol was removed by distillation under reduced pressure; the residue was taken up into ethyl acetate (250 ml) under reflux, filtered hot, the filter cake washed with warm ethyl acetate (100 ml). The combined filtrate was cooled to −10° C., aged for 1.5 hours. The precipitate was collected, washed twice with cold ethyl acetate (2×25 ml), dried to give N-benzyl-4-hydroxy-3-oxobutanamide (18.2 g, 101 mmol, 38.8% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09346751B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-75d1eb007b04441f8953c1e8edbc0291 |
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| 出典メモ | uspto-grants-2016_05 |
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