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Diethyl Oxalate → Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Oxalate | HCID 7268 | — |
| 反応物 | Ethanone, 1-(2,4,6-trimethylphenyl)- | HCID 15461 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl 2,4-dioxo-4-(2,4,6-trimethylphenyl)butanoate | HCID 14945000 | 66.7% |
反応手順
To a solution of 2', 4', 6'-trimethylacetophenone (15 g, 92.6 mmol) and diethyl oxalate (20 g, 139 mmol) in 500 mL of anhydrous toluene was cautiously added 7.4 g of NaH (60% dispersion in mineral oil). The reaction mixture was slowly heated to reflux under N2. It was refluxed for about 20 minutes, then cooled, poured into ice-cold aqueous HCl solution, and extracted with ether. The extracts were washed with brine, dried over Na2SO4, filtered through a short silica gel pad and concentrated to give 16.2 g of a red oil which was used in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723608 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-54fc6a8a376c4fd9a41d798a9116e90e |
| 出典メモ | uspto-grants-1998_03 |