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Sodium Hydroxide → 6-(Oxiran-2-yl)-2,3-dihydro-1,4-benzodioxine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Formyl-1,4-benzodioxane | HCID 191725 | — |
| 反応物 | Trimethylsulfonium methyl sulfate | HCID 2760871 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-(Oxiran-2-yl)-2,3-dihydro-1,4-benzodioxine | HCID 16781333 | 100.7% |
反応手順
A mixture of 1,4-benzodioxanecarboxaldehyde [RN 29668-44-8](1.5 g, 9.14 mmol), trimethylsulfonium methyl sulfate (2.24 g, 11.9 mmol), dichloromethane (35 ml) and 50% aqueous sodium hydroxide (5 ml) were vigorously stirred for 70 hours. The mixture was partitioned between water and diethyl ether and the layers separated. The aqueous phase was extracted with diethyl ether. The combined organic phases were washed with water, brine, then dried over magnesium sulfate and evaporated to give crude 6-oxiranyl-2,3-dihydro-benzo[1,4]dioxine (1.64 g, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07186730B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-6c474692bdbe4f82b3b6d1648d1a2bc8 |
| 出典メモ | uspto-grants-2007_03 |