반응식
Cl.[C:2]1([S:8][CH2:9][CH2:10][NH:11][CH:12]([CH3:14])[CH3:13])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.B1([O-])O[O:16]1.[OH2:19].[OH2:20].[OH2:21].[OH2:22].[Na+].[OH-].[Na+]>S(=O)(=O)(O)O>[C:2]([OH:22])(=[O:21])/[CH:3]=[CH:4]\[C:5]([OH:20])=[O:19].[C:2]1([S:8]([CH2:9][CH2:10][NH:11][CH:12]([CH3:14])[CH3:13])=[O:16])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1참가 물질
5
실험 절차
A solution of 15.62 g (0.067 mole) of N-[2-(phenylthio)ethyl]-2-propanamine hydrochloride and 15.62 g (0.101 mole) of sodium perborate tetrahydrate in 300 ml of 2M sulfuric acid was stirred at room temperature for 16 hr. The solution was made basic with 50% sodium hydroxide, and the basic solution was extracted with methylene chloride. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in ether, a solution of maleic acid in methanol was added, and precipitated to give 19.48 g (88.3%) of white solid, m.p. 102.5°-103.5° C. A sample of this was recrystallized from methanol-ether, m.p. 102.5°-103.5° C.
후처리
- extractionthe basic solution was extracted with methylene chloride
- dry with materialThe methylene chloride solution was dried over magnesium sulfate
- customthe solvent was removed in vacuo
- dissolutionThe residue was dissolved in ether
- additiona solution of maleic acid in methanol was added
- customprecipitated
출처 및 근거
- ORD 기록
- ord-df95688818af431f92f3b925fa45e917
- 출처 데이터셋
- uspto-grants-1988_02
- 특허 번호
- US04724235
연결된 노트
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