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Boron tribromide → 2-Bromo-1-(3,4-dihydroxy-5-nitro-phenyl)-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Boron tribromide | HCID 25134 | — |
| 反応物 | 2-Bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone | HCID 14450983 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Bromo-1-(3,4-dihydroxy-5-nitro-phenyl)-ethanone | HCID 21845596 | — |
反応手順
A suspension of 29.0 g of 2-bromo-4'-hydroxy-3'-methoxy-5'-nitroacetophenone in 700 ml of dry methylene chloride is treated at -20° within 30 minutes with a solution of 125.3 g of boron tribromide in 300 ml of dry methylene chloride. After the addition the mixture is stirred at -20° for a further 1 hour and at room temperature for 16 hours, then evaporated, the residue is treated cautiously with water while cooling with ice and stirred at 50° for 30 minutes. After cooling the mixture is extracted with ether, the ethereal phase is washed with water, dried over sodium sulfate, filtered and evaporated. There is obtained 2-bromo-3',4'-dihydroxy-5'-nitroacetophenone of m.p. 138°-140° (from methylene chloride).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05389653 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-41984e31f2db426abf9494899f940258 |
| 出典メモ | uspto-grants-1995_02 |