Dimethyl Sulfate → HCID 10773603, 화합물

HRID 2075537노트

반응식

HRID 2075537 반응식
[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([OH:12])=[CH:4][CH:3]=1.[C:13](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([O:12][CH3:13])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 109208304-fluoronaphthalen-1-ol

생성물 1

HCID 10773603HCID 10773603, 화합물수율 48.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

21.7 g of 4-Fluoro-naphthalen-1-ol were dissolved in 250 mL acetone. 39.0 g of potassium carbonate and 14.6 mL dimethyl sulfate were added at room temperature. The reaction was placed under nitrogen and stirred for 72 h. The mixture was filtrated, the solid washed with acetone, and the filtrate was concentrated to a viscous oil, which was taken up in ethyl acetate. This was washed with water and with brine, dried over sodium sulfate, filtered through celite and concentrated. The resulting oil was distilled using a Kugelrohr-apparatus, yielding 11.4 g of 4-fluoro-1-methoxynaphthalene.

후처리

  1. filtrationThe mixture was filtrated
  2. washthe solid washed with acetone
  3. concentrationthe filtrate was concentrated to a viscous oil, which
  4. washThis was washed with water and with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered through celite and
  7. concentrationconcentrated
  8. distillationThe resulting oil was distilled

출처 및 근거

ORD 기록
ord-073114ebc1f44766a87b60e26ce99a4d
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919628B2

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