反応式
[Br:1][C:2]1[CH:6]=[CH:5][S:4][CH:3]=1.[CH3:7][CH:8]1OC(C)OC(C)O1.[CH:16]([C:19]1[CH:27]=[CH:26][C:22]([C:23]([NH2:25])=[O:24])=[CH:21][CH:20]=1)([CH3:18])[CH3:17].P(=O)(O)(O)O>O.C(O)=O>[Br:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]([NH:25][C:23](=[O:24])[C:22]1[CH:26]=[CH:27][C:19]([CH:16]([CH3:18])[CH3:17])=[CH:20][CH:21]=1)[CH3:8]参加物
7
実験手順
3-Bromothiophene (8.15 g, 0.05 mol), paraldehyde (2.20 g, 0.017 mol) and 4-isopropylbenzamide (1.63 g, 0.01 mol) were added to a mixture of formic acid (6 ml) and 85% phosphoric acid (3 ml) and stirred at a room temperature for four hours. Water (50 ml) was added to the reaction mixture. The mixture was extracted with chloroform (50 ml), subjected to a silica gel column chromatography (eluent: chloroform) and recrystallized from chloroform/petroleum benzine (1:2) to obtain the entitled compound (0.6 g) as a colorless plate-shape crystal. Yield: 17.0%. Melting point: 133° C.
後処理
- extractionThe mixture was extracted with chloroform (50 ml)
- customrecrystallized from chloroform/petroleum benzine (1:2)
出典と根拠
- ORDレコード
- ord-8cad702cee3f4bffbf519ecb8a9ea6de
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05117000
関連ノート
読み込み中…