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Diethyl Ether → 1,5-Dihydro-3-methoxy-2,4-benzodioxepin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 1,2-Benzenedimethanol | HCID 69153 | — |
| 反応物 | 3-(1-propenyl)-1,5-dihydro-3H-2,4-benzodioxepine | HCID 53720123 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 1,5-Dihydro-3-methoxy-2,4-benzodioxepin | HCID 3795208 | 89% |
反応手順
A method for synthesizing 3-(1-propenyl)-1,5-dihydro-3H-2,4-benzodioxepine is illustrated in Scheme 3. 1,2-Benzenedimethanol (500 mg, 3.62 mmol) and p-toluenesulfonic acid (172 mg, 0.9 mmol) were dissolved in 2 mL of dry DME and triethylortoformate (0.396 mL, 3.62 mmol) was added. The solution was stirred at rt. and under argon for 1 h. Ether (20 mL) was added and the organic layer washed with a saturated solution of NaHCO3 and water, then dried (Na2SO4). The solvent was evaporated giving crude 3-methoxy-1,5-dihydro-3H-2,4 benzodioxepine as a colorless oil (526 mg, 89%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713287B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-6acbabc4189d4bf5b0e7c53207e55958 |
| 出典メモ | uspto-grants-2004_03 |