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Methanol → 1,2-Bis(3,4-dihydroxyphenyl)ethane-1,2-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 1,2-Bis(1,3-benzodioxol-5-yl)ethane-1,2-dione | HCID 226339 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,2-Bis(3,4-dihydroxyphenyl)ethane-1,2-dione | HCID 238232 | 47.2% |
反応手順
To a stirred solution of bis(3,4-methylenedioxy)benzil (500 mg) in dry CH2Cl2 (50 ml) under nitrogen, was slowly added boron tribromide (1.6 ml) then stirring continued for a further 3.5 hours. Methanol (100 ml) was added carefully, then the solvent evaporated in vacuo to a volume of 1 ml, this addition and evaporation was repeated twice more. The product was purified by column chromatography over silica gel when elution with diethylether in dichloromethane gave 3,4,3′,4′-tetrahydroxybenzil (217 mg, 47%) as a yellow powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07514583B2 |
| 出典データセット | uspto-grants-2009_04 |
| ORD ID | ord-e658ef01f62f4b5c8a713a50ab81ba01 |
| 出典メモ | uspto-grants-2009_04 |