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Carbon Disulfide → 5-Bromo-2,4-dimethoxyphenol

HRID 1457594
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HRID 1457594 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][C:4]=1[OH:11].C(=S)=S.[Br:15]Br>O>[Br:15][C:6]1[CH:5]=[C:4]([OH:11])[C:3]([O:2][CH3:1])=[CH:8][C:7]=1[O:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6348Carbon DisulfideHCID 24408BromineHCID 5930062,4-Dimethoxyphenol

생성물 1

HCID 220994575-Bromo-2,4-dimethoxyphenol수율 92%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixed solution comprising 8.6 g of 2,4-dimethoxyphenol and 80 ml of carbon disulfide (CS2) was added dropwise 2.86 ml of bromine at 10° to 15° C. After stirring the mixture at room temperature for one hour, water was added to the reaction mixture and the reaction mixture was extracted with diethyl ether. The extract was washed and dried, and the solvent was removed under reduced pressure. Hexane was added to the obtained residue and the precipitated crystals were collected by filtration to give 12.0 g of 3-bromo-4,6-dimethoxyphenol (yield: 92%, melting point: 78°-80° C.).

후처리

  1. extractionthe reaction mixture was extracted with diethyl ether
  2. washThe extract was washed
  3. customdried
  4. customthe solvent was removed under reduced pressure
  5. additionHexane was added to the obtained residue
  6. filtrationthe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-019c909aa59c45e6912ff3b83990ce73
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849732

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