関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2-Ethyl-1,3-Hexanediol | HCID 7211 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | Phosphoric acid, disodium salt, dodecahydrate | HCID 61456 | — |
| 触媒 | Sodium Tungstate Dihydrate | HCID 150191 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | 2-Ethyl-1-hydroxy-3-hexanone | HCID 11116179 | — |
反応手順
Into 5.90 g of 35% hydrogen peroxide solution (60.0 mmol), 720 mg of disodium phosphate dodecahydrate (2.0 mmol) and 165 mg of sodium tungstate dihydrate (0.5 mmol) were dissolved to prepare a mixed reagent (pH 6.5). After 7.3 g of 2-ethyl-1,3-hexanediol (50.0 mmol) was dissolved into 100 mL of N,N-dimethylacetamide, the resultant was heated to 90° C., and the above mixed reagent was added. After the reaction was continued at 90° C. for four hours, 100 mL of toluene and 100 g of 10% brine were added for liquid separation. The aqueous layer was extracted three times with 100 mL of toluene, and all the organic layers were combined and concentrated under reduced pressure. The concentrated liquid was separated and purified by silica gel chromatography (developing solvent hexane:ethyl acetate=3:2) to obtain oily 2-ethyl-1-hydroxy-3-hexanone. The yield was 5.33 g (73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08017793B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-85edff2eb09a47ca976ed5f7cb9545a4 |
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| 出典メモ | uspto-grants-2011_09 |
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