反応式
[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].C(#N)C.[C:12](O)(=[O:14])[CH3:13]>C(OCC)(=O)C>[Br:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH:4][C:12](=[O:14])[CH3:13]参加物
5
実験手順
2-Bromo-1-acetylaminobenzene was synthesized in the usual manner from 2-bromoaniline. That is, 150 ml of acetonitrile was added to 25.0 g of 2-bromoaniline, then 15.1 ml of glacial acetic acid was added thereto, and the reaction mixture was heated under reflux for 2 hours. After bringing its temperature to room temperature, 300 ml of ethyl acetate was added thereto, and after the resulting mixture was washed with water twice, the solvent was distilled off, and recrystallization of the crude crystals from a hexane/ethyl acetate solvent mixture was carried out, to obtain 23.2 g (yield: 75%) of 2-bromo-1-acetylaminobenzene.
後処理
- temperaturethe reaction mixture was heated
- temperatureunder reflux for 2 hours
- customto room temperature
- washafter the resulting mixture was washed with water twice
- distillationthe solvent was distilled off
- customrecrystallization of the crude crystals from a hexane/ethyl acetate solvent mixture
出典と根拠
- ORDレコード
- ord-5591e418656b4c909c222813e8b51adb
- 出典データセット
- uspto-grants-1991_04
- 特許番号
- US05006660
関連ノート
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