関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,3-Dibromopropanoyl chloride | HCID 86790 | — |
| 反応物 | N-Isopropylhydroxylamineoxalate | HCID 19871111 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 19871100 | HCID 19871100 | 63.4% |
反応手順
To a stirred mixture of 6 g (25 mmol) of N-isopropylhydroxylamine oxalate and 1N sodium hydroxide (50 ml) in water (100 ml) cooled to 0° C. there was added 2,3-dibromopropionyl chloride (12.5 g, 50 mmol), followed by the addition of 50 ml of 1N sodium hydroxide. Ten minutes later, 150 ml of methylene chloride and 60 ml of 1N sodium hydroxide were added. The mixture was stirred continuously for one hours following which the organic phase was separated, dried over anhydrous magnesium sulfate and concentrated. The concentrate was chromatographed on silica gel with 40% ethyl acetatehexane to afford 3.3 g of 4-bromo-2-isopropyl-3-isoxazolidinone.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04892870 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-730eb489b9ec4f098361805efb92dc25 |
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| 出典メモ | uspto-grants-1990_01 |
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