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Triethylamine → 2,2-Difluoro-5-methoxypentan-1-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trimethylsilyl iodide | HCID 85247 | — |
| 反応物 | 2,2-Difluoro-1-benzyloxy-5-methoxypentane | HCID 20149494 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-Difluoro-5-methoxypentan-1-ol | HCID 14097599 | 67.9% |
反応手順
Trimethylsilyliodide (5.2 g, 26 mmoles) is added to a solution of 2,2-difluoro-1-benzyloxy-5-methoxypentane (6.3 g, 25.8 mmoles) in dry dichloromethane (30 ml), kept under nitrogen at room temperature. After standing for 1 hour at 25° C., the reaction mixture is treated with triethylamine (5 ml) during 1 hour, diluted with dichloromethane and washed with 1N HCl and twice with diluted brine. Bulb to bulb distillation of the crude oil obtained (4.2 g) (110°-150° C., 15 mm) gives the title compound (2.7 g, contaminated with 10% of 2,2-difluoro-1-benzyloxy-5-hydroxy pentane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04730006 |
| 出典データセット | uspto-grants-1988_03 |
| ORD ID | ord-34a24940a15c47168cff0f4638222e1b |
| 出典メモ | uspto-grants-1988_03 |