Phosphorus pentachloride → N-(2,6-dichlorophenyl)-2,3-dihydro-2-oxothieno[3,4-b]pyrrole
반응식
[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]12참가 물질
4
실험 절차
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°).
후처리
- extractionThe mixture is extracted with water and sodium bicarbonate solution
- concentrationconcentrated
- customRecrystallization of the residue from isopropanol
출처 및 근거
- ORD 기록
- ord-142fa22fbd3b4f498e995f2f7de0a3d6
- 출처 데이터셋
- uspto-grants-1981_06
- 특허 번호
- US04272507
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