반응식
[C:1]([N:9]1[CH2:13][CH:12]=[CH:11][CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:14][S:15](Cl)(=O)=O.[NH3:19].C(=O)([O-])[O-].[Na+].[Na+]>O1CCCC1.O.C(Cl)Cl>[C:1]([N:9]1[CH2:13][C@@H:12]([S:15][CH3:14])[C@H:11]([NH2:19])[CH2:10]1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
실험 절차
41.5 g (0.24 mol) of 1-benzoyl-2,5-dihydropyrrole are initially introduced into 240 ml of methylene chloride, and 24.8 g (0.3 mol) of methanesulphonyl chloride are added dropwise at 0° C. The mixture is subsequently stirred at room temperature for 16 hours, the solvent is then stripped off under 8 mbar and the residue is taken up in 240 ml of tetrahydrofuran. After addition of 65 g of 25% strength ammonia solution, the mixture is heated at 80° C. in an autoclave for 10 hours. It is then poured into 5 times the amount of water, the pH is brought to 10-11 with sodium carbonate, the mixture is extracted with methylene chloride and the extract is dried over sodium sulphate and concentrated. The crude product (50 g) is chromatographed on silica gel (mobile phase initially ethanol:ethyl acetate 1:3, then ethanol; Rf value: 0.34 ethanol). Yield: 33.5 g (59% of theory).
후처리
- additionare added dropwise at 0° C
- temperaturethe mixture is heated at 80° C. in an autoclave for 10 hours
- extractionthe mixture is extracted with methylene chloride
- dry with materialthe extract is dried over sodium sulphate
- concentrationconcentrated
- customThe crude product (50 g) is chromatographed on silica gel (mobile phase initially ethanol:ethyl acetate 1:3
출처 및 근거
- ORD 기록
- ord-0261170fe1524559b435f9b568c4bc3a
- 출처 데이터셋
- uspto-grants-1991_10
- 특허 번호
- US05061712
연결된 노트
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