反応式
C(N(CC)CC)C.[Br:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1.[C:16](Cl)(=[O:19])[CH2:17][CH3:18].O>CN(C)C1C=CN=CC=1.ClCCl>[C:16]([O:15][C:12]1[CH:13]=[CH:14][C:9]([Br:8])=[CH:10][CH:11]=1)(=[O:19])[CH2:17][CH3:18]参加物
7
実験手順
Triethylamine (219 ml) was added to a solution of 4-bromophenol (259 g) and 4-dimethylaminopyridine (1.5 g) in dichloromethane (1000 ml) at 0° C. at such a rate that the temperature did not rise above 20° C. When the addition was complete propionyl chloride (137 ml) was added in portions over 1 hour such that the temperature did not rise above 20° C. Finally, the mixture was stirred at room temperature for 2 hours. Water (700 ml) was added and the layers were separated. The dichloromethane solution was washed with brine (500 ml), dried (MgSO4) and concentrated in vacuo to give the title compound as an oil, 344 g.
後処理
- customdid not rise above 20° C
- additionWhen the addition
- additionwas added in portions over 1 hour such that the temperature
- customdid not rise above 20° C
- customthe layers were separated
- washThe dichloromethane solution was washed with brine (500 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-18e97558a3014f24875cdb5f4e4d3b20
- 出典データセット
- uspto-grants-1997_10
- 特許番号
- US05677324
関連ノート
読み込み中…