反応式
[CH2:1](Br)[C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:3].[CH3:11][CH2:12][O:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([NH2:20])[CH:15]=1.C([O-])([O-])=O.[Na+].[Na+]>C(O)C>[CH2:12]([O:13][C:14]1[CH:15]=[C:16]([NH:20][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:2](=[O:3])[CH3:1])[CH:17]=[CH:18][CH:19]=1)[CH3:11]参加物
5
実験手順
5 g of phenacyl bromide and 3.78 g of m-phenetidine are stirred at 50° C. for 2.5 h in 50 ml of ethanol in the presence of 5.85 g of powdered Na2CO3. The mixture is then cooled and concentrated in an RE. The residue is partitioned between water and methylene chloride and the aqueous phase is extracted twice with methylene chloride. The combined organic phases are dried over Na2SO4 and concentrated. The residue is slurried with ether and the crystals are filtered off, 2'-(3-ethoxyphenylamino)acetophenone being obtained. Further product is again obtained from the mother liquor after addition of petroleum ether.
後処理
- temperatureThe mixture is then cooled
- concentrationconcentrated in an RE
- customThe residue is partitioned between water and methylene chloride
- extractionthe aqueous phase is extracted twice with methylene chloride
- dry with materialThe combined organic phases are dried over Na2SO4
- concentrationconcentrated
- filtrationthe crystals are filtered off
出典と根拠
- ORDレコード
- ord-a4c2f8e276d2461884398f346404e01b
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05869485
関連ノート
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