Hydrochloric Acid → 2-Chloro-3-methoxyphenol

HRID 629378

반응식

HRID 629378 반응식
[Cl:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9].S(OC)(O[CH3:14])(=O)=O.Cl>[OH-].[K+]>[Cl:1][C:2]1[C:7]([O:8][CH3:14])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:9]

참가 물질

5

반응 조건

온도
100 °C

실험 절차

To an aqueous solution (100 mL) of potassium hydroxide (11.0 g) was added 2-chlorobenzene-1,3-diol (22.8 g). Then, dimethyl sulfate (19.9 g) was slowly added to the reaction mixture while keeping the reaction mixture at 10° C. to 20° C., and the mixture was stirred at 100° C. for 2 days. The reaction mixture was acidified with 2N hydrochloric acid, and the mixture was extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether) to give the title compound (18.0 g).

후처리

  1. customat 10° C. to 20° C.
  2. extractionthe mixture was extracted with dichloromethane
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/petroleum ether)

출처 및 근거

ORD 기록
ord-60c19c208b704da8ac733c8b083c62bd
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315458B2

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