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2-Bromo-1-(3,4-dichlorophenyl)ethanone → 1-(3,4-Dichlorophenyl)-2-hydroxyethan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-1-(3,4-dichlorophenyl)ethanone | HCID 244751 | — |
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-(3,4-Dichlorophenyl)-2-hydroxyethan-1-one | HCID 7062193 | 42% |
反応手順
A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 ml) was stirred with heating under reflux for 16 hours. The reaction mixture was concentrated and poured into water (1 L). The solid precipitates were filtered, washed with water and then isopropyl ether, and air-dried. The residue was dried under reduced pressure to give crystals of 2-hydroxy-3′,4′-dichloroacetophenone (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale yellow prisms. Melting point 115-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07396848B1 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-890678fea6054182989fef150ca76d42 |
| 出典メモ | uspto-grants-2008_07 |