化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2-(Bromomethyl)-5-(difluoromethoxy)-1,3-difluorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro- | HCID 69140944 | — |
| 生成物 | 2-(Bromomethyl)-5-(difluoromethoxy)-1,3-difluorobenzene | HCID 86732431 | — |
反応手順
0.76 g of [4-(difluoromethoxy)-2,6-difluorophenyl]methanol (3.62 mmol, 1 eq.) were dissolved in 1.72 ml of 33% hydrogen bromide in glacial acetic acid (9.97 mmol, 2.75 eq.) and stirred at room temperature for 2 hours. 25 ml of diethyl ether were added and the mixture was stirred at room temperature for 15 min. The reaction mixture was added dropwise to 80 ml of aqueous saturated sodium hydrogen carbonate solution and stirred again at room temperature for 15 min. The separated aqueous layer was extracted twice with diethyl ether. The combined organic layers were washed with brine, dried over a silicone filter and concentrated in vacuo to yield 991 mg (3.56 mmol, 98.4%) of the analytically pure target compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09265763B2 |
| 出典データセット | uspto-grants-2016_02 |
| ORD ID | ord-a40a61c28124466a8b14d8a1492bdff5 |
| 出典メモ | uspto-grants-2016_02 |