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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 heated under reflux and stirred for 16 h. The reaction mixture was concentrated and poured into water (1 L). The precipitated solid was collected by filtration, washed with water and then with isopropyl ether, air-dried, and further dried under reduced pressure at 40° C. to give the title compound as crystals (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 115-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06699995B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-3bf23ac72d0e454e87c0e21c7a1e4332 |
| 出典メモ | uspto-grants-2004_03 |