関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl hydroperoxide | HCID 6410 | — |
| 反応物 | Ethyl 6-ethyl-2,3-dihydro-1,4-benzodioxin-2-carboxylate | HCID 15210220 | — |
| 触媒 | chromium (VI) trioxide | HCID 10219390 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 6-acetyl-2,3-dihydro-1,4-benzodioxine-2-carboxylate | HCID 15210221 | 62% |
反応手順
Add 2 g (8.5 mmol) of ethyl 6-ethyl-2,3-dihydro-1,4-benzodioxin-2-carboxylate dissolved in 5 cm3 of anhydrous methylene chloride to a mixture at 0° C. of 0.042 g (0.42 mmol) of chromium trioxide and 5.35 g (59.3 mmol) of 70% tert-butyl hydroperoxide in 30 cm3 of methylene chloride. Stir for 2 hours at 0° C. and then for 72 hours at room temperature. The crude product obtained by concentrating to dryness is purified by chromatography on a silica column (eluant: methylene chloride). Ethyl 6-acetyl-2,3-dihydro-1,4-benzodioxin-2-carboxylate is thereby obtained in a yield of 62%. Melting point: 60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05439909 |
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| 出典データセット | uspto-grants-1995_08 |
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| ORD ID | ord-d687941ae6164db7abd9fc2137968029 |
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| 出典メモ | uspto-grants-1995_08 |
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