p-Toluenesulfonic acid monohydrate → HCID 136335928、化合物
反応式
[NH2:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[CH:6][C:7]=1[Cl:8].[Cl:10][C:11]1[CH:24]=[CH:23][C:14]([O:15][CH:16]([C:20](=O)[CH3:21])[C:17](=O)[CH3:18])=[CH:13][CH:12]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>>[Cl:8][C:7]1[C:2]2[N:1]=[C:20]([CH3:21])[C:16]([O:15][C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:24][CH:23]=3)=[C:17]([CH3:18])[C:3]=2[C:4]([OH:9])=[CH:5][CH:6]=1参加物
4
反応条件
- 温度
- 125 °C
実験手順
A mixture of 3-amino-4-chlorophenol (0.36 g), 3-(4-chlorophenoxy)pentane-2,4-dione (0.57 g) and p-toluenesulfonic acid monohydrate (0.020 g) was heated at 125° C. for 3 hours. The mixture was cooled to room temperature and purified by column chromatography on silica gel, eluting with a mixture of dichloromethane and ethyl acetate (1:0 to 0:1 by volume) to afford title compound as a brown oil, 0.16 g.
後処理
- temperatureThe mixture was cooled to room temperature
- custompurified by column chromatography on silica gel
- washeluting with a mixture of dichloromethane and ethyl acetate (1:0 to 0:1 by volume)
出典と根拠
- ORDレコード
- ord-d0597e3960964cdc9546e0718bc6934e
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07858640B2
反応ノート
読み込み中…