反応式
[Br:1]Br.[C:3]([NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13](=[O:15])[CH3:14])(=[O:5])[CH3:4]>C(Cl)(Cl)Cl>[C:3]([NH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13](=[O:15])[CH2:14][Br:1])(=[O:5])[CH3:4]参加物
4
実験手順
45.0 g (0.282 mol) of dry bromine were added dropwise to a boiling solution of 50.0 g (0.282 mol) of 1-[2-(acetylamino)phenyl]ethanone in 400 ml of chloroform at room temperature. The solvent was distilled off, the residue was distributed between dichloromethane and saturated ice-cold sodium hydrogen carbonate solution. The organic phase was dried over sodium sulphate, evaporated down in vacuo, the residue was triturated with diethylether and suction filtered. After drying in vacuo 35.4 g (49% of theory) of colourless crystals were obtained, Rf=0.48 (eluant: petroleum ether/ethyl acetate 2/1 v/v).
後処理
- distillationThe solvent was distilled off
- dry with materialThe organic phase was dried over sodium sulphate
- customevaporated down in vacuo
- customthe residue was triturated with diethylether and suction
- filtrationfiltered
- customAfter drying in vacuo 35.4 g (49% of theory) of colourless crystals
- customwere obtained
出典と根拠
- ORDレコード
- ord-926f7b0a23cc4338b77caa0fd2afa495
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07498325B2
関連ノート
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