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Dimethyl Sulfate → 2-Methoxy-3-(2-chlorophenylthio)benzaldehyde

HRID 1164078
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HRID 1164078 반응식
[OH:1][C:2]1[C:9]([S:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].S(OC)(O[CH3:22])(=O)=O>[OH-].[K+]>[CH3:22][O:1][C:2]1[C:9]([S:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6497Dimethyl SulfateHCID 205134432-Hydroxy-3-(2-chlorophenylthio)benzaldehyde

생성물 1

HCID 205134222-Methoxy-3-(2-chlorophenylthio)benzaldehyde수율 45.3%

시약·촉매·용매 1

HCID 14797Potassium Hydroxide용매

실험 절차

A mixture of 2-hydroxy-3-(2-chlorophenylthio)benzaldehyde (19.3 g) and dimethyl sulfate (18.4 g) was stirred at room temperature. To the mixture was added dropwise an aqueous solution (50 ml) of potassium hydroxide (12.5 g) at temperature below 60° C., and then the mixture was stirred for an hour. The reaction mixture was cooled to the ambient temperature and insoluble substance was filtered off. The filtrate was extracted with diethyl ether, and the extract was washed with water, dried over magnesium sulfate and then evaporated under reduced pressure to give oily 2-methoxy-3-(2-chlorophenylthio)benzaldehyde (9.2 g).

후처리

  1. stirringthe mixture was stirred for an hour
  2. temperatureThe reaction mixture was cooled to the ambient temperature and insoluble substance
  3. filtrationwas filtered off
  4. extractionThe filtrate was extracted with diethyl ether
  5. washthe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-8fd23be2987848789d8e31e8d523dfd2
출처 데이터셋
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04367238

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