Sulfuric Acid → 2,3-Dichloro-4-methoxybenzene-1-thiol
반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[S:11](Cl)(=O)=O.S(=O)(=O)(O)O>ClCCl.[Zn]>[Cl:1][C:2]1[C:7]([Cl:8])=[C:6]([O:9][CH3:10])[CH:5]=[CH:4][C:3]=1[SH:11]참가 물질
5
실험 절차
A mixture of 9.37 g of 2,3-dichloro-4-methoxybenzenesulfonyl chloride, 72 g of crushed ice, 24 g of conc. sulfuric acid and 12 g of zinc dust is stirred under reflux for 16 hours. The mixture is diluted with dichloromethane, cooled and stirred at room temperature for 2 hours. Filtration removes the unreacted zinc and the organic extracts are washed with water, sodium bicarbonate solution and dried over anhydrous magnesium sulfate. Removal of solvent in vacuo leaves a white solid which is recrystallized from ether-pentane to give 5.5 g of 2,3-dichloro-4-methoxy-thiophenol as colorless needles, mp 81.5°-83°.
후처리
- temperatureunder reflux for 16 hours
- temperaturecooled
- stirringstirred at room temperature for 2 hours
- filtrationFiltration
- customremoves the unreacted zinc
- washthe organic extracts are washed with water, sodium bicarbonate solution
- dry with materialdried over anhydrous magnesium sulfate
- customRemoval of solvent in vacuo
- customleaves a white solid which
- customis recrystallized from ether-pentane
출처 및 근거
- ORD 기록
- ord-da599bf63eb548538e475c168cea25c8
- 출처 데이터셋
- uspto-grants-1985_07
- 특허 번호
- US04528399
반응 노트
불러오는 중…