반응식
Br.[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3].C(N(CC)CC)C>CO>[ClH:16].[CH2:2]([N:4]1[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([S:17](=[O:20])(=[O:19])[NH2:18])[CH:11]=2)([OH:9])[CH2:7][S:6][C:5]1=[N:21][CH2:22][CH3:23])[CH3:3]참가 물질
4
반응 조건
- 온도
- 40 °C
실험 절차
17 g of 3-ethyl-2-ethylimino-4-(4-chloro-3-sulfamoylphenyl)-1,3-thiazolidine-4-ol-hydrobromide were suspensed in 100 ml of methanol and shortly heated to boiling after the addition of 10 ml of triethyl amine. The solvent was distilled off under reduced pressure, 150 ml of water were added to the residue and the mixture was extracted with 200 ml of ethyl acetate. After drying the organic phase over sodium sulfate the solvent was distilled off under reduced pressure. The residue was dissolved in 100 ml of acetone, the solution was acidified with 15% ethanolic HCl and the oily precipitate of the end product was crystallized with acetone heated to 40° C. Melting point: 177° C. (decomposition).
후처리
- temperatureshortly heated
- distillationThe solvent was distilled off under reduced pressure, 150 ml of water
- additionwere added to the residue
- extractionthe mixture was extracted with 200 ml of ethyl acetate
- dry with materialAfter drying the organic phase over sodium sulfate the solvent
- distillationwas distilled off under reduced pressure
- dissolutionThe residue was dissolved in 100 ml of acetone
- customthe oily precipitate of the end product was crystallized with acetone
출처 및 근거
- ORD 기록
- ord-5eb6cd53d8b84e60833fef1ab9224fd7
- 출처 데이터셋
- uspto-grants-1978_11
- 특허 번호
- US04125614
연결된 노트
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