Phosphorus pentachloride → N-(2,6-dichlorophenyl)-2,3-dihydro-2-oxothieno[3,4-b]pyrrole
反応式
[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[C:3]=1[NH:4][C:5]1[C:6]([CH2:10][C:11](O)=[O:12])=[CH:7][S:8][CH:9]=1.P(Cl)(Cl)(Cl)(Cl)Cl>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[C:3]=1[N:4]1[C:11](=[O:12])[CH2:10][C:6]2=[CH:7][S:8][CH:9]=[C:5]12参加物
4
実験手順
1 g (0.33 mmole) of 4-(2,6-dichloroanilino)-3-thiophenacetic acid and 0.7 g (0.33 mmole) of phosphorus pentachloride are stirred in 10 ml of toluene at room temperature for half an hour. The mixture is extracted with water and sodium bicarbonate solution, clarified with bleaching earth (for example Tonsil®) and concentrated. Recrystallization of the residue from isopropanol yields N-(2,6-dichlorophenyl)-2,3-dihydro-2-oxothieno[3,4-b]pyrrole (m. 187° to 188°).
後処理
- extractionThe mixture is extracted with water and sodium bicarbonate solution
- concentrationconcentrated
- customRecrystallization of the residue from isopropanol
出典と根拠
- ORDレコード
- ord-142fa22fbd3b4f498e995f2f7de0a3d6
- 出典データセット
- uspto-grants-1981_06
- 特許番号
- US04272507
反応ノート
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