化工社化工社 化学情報印刷レポート · 研究参考用
Methyl iodide → Methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,3-Dihydro-1,4-benzodioxin-6-ol | HCID 9115273 | — |
| 触媒 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine | HCID 21624819 | 85% |
反応手順
To a mixture of K2CO3 (47.54 g, 344 mmol) and Bu4NI (1.256 g, 3.4 mmol) in DMF was added 2,3-dihydro-benzo[1,4]dioxin-6-ol (26.2 g, 172 mmol) followed by iodomethane (16.1 ml, 258 mmol). After 16 hours the mixture was filtered. The solution was mixed with H2O and extracted with ethyl acetate. The combined organics were washed with brine, dried over MgSO4, filtered and concentrated in vacuo. Purification via flash chromatography (95:5 hexane/ethyl acetate) afforded methyl 6-methoxy-2,3-dihydro-benzo[1,4]dioxine (24.23 g, 85%) as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846705B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-4e61b2e136dd4c8196edbfa0894d4da2 |
| 出典メモ | uspto-grants-2014_09 |