反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1.C1C=C[NH+:14]=CC=1.[Br:17][Br-]Br>C(O)(=O)C>[ClH:1].[NH2:14][CH2:9][C:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)=[O:10].[Br:17][CH2:9][C:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)=[O:10]参加物
4
実験手順
The starting 2-amino-1-(4-chlorophenyl)ethanone hydrochloride was prepared according to the following procedure. The 1-(4-chlorophenyl)ethanone (1.0 eq.) was dissolved in glacial acetic acid (1 ml, per mmol). To this was added a slurry of pyridinium bromide perbromide (1.03 eq.) in acetic acid (1 mL per mmol). The heterogeneous mixture was stirred for 4 h at ambient temperature. After about 30 min. the mixture turned homogeneous. After pouring into ice-water a yellow precipitate was filtered off and washed with water (2×1 mL per mmol of starting ketone). Drying of the precipitate afforded 2-bromo-1-(4-chlorophenyl)ethanone in ca. 90% yield.
後処理
- waitAfter about 30 min. the mixture turned homogeneous
- filtrationwas filtered off
- washwashed with water (2×1 mL per mmol of starting ketone)
- customDrying of the precipitate
出典と根拠
- ORDレコード
- ord-c36b39ac91384ba699e4e403ccd48175
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08017555B2
関連ノート
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