Dimethyl Sulfate → 4-Fluoro-7-methoxy-2,3-dihydro-1H-inden-1-one

HRID 1492955노트

반응식

HRID 1492955 반응식
[C:1](=O)([O-])[O-].[K+].[K+].[F:7][C:8]1[CH:16]=[CH:15][C:14]([OH:17])=[C:13]2[C:9]=1[CH2:10][CH2:11][C:12]2=[O:18].S(OC)(OC)(=O)=O>CC(C)=O>[F:7][C:8]1[CH:16]=[CH:15][C:14]([O:17][CH3:1])=[C:13]2[C:9]=1[CH2:10][CH2:11][C:12]2=[O:18]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 152684884-Fluoro-7-hydroxy-2,3-dihydro-1H-inden-1-one

생성물 1

HCID 146450284-Fluoro-7-methoxy-2,3-dihydro-1H-inden-1-one

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

In a nitrogen atmosphere, to 300 g powdered potassium carbonate in 1.5 1 of acetone is added 121 g II under stirring, followed by 83 ml of dimethyl sulphate. After heating to reflux for 2 hrs, the solvent is distilled off, water is added and the mixture refluxed for a further hour. Extraction with methylene chloride and evaporation gives 125 g of crude III, which is purified by crystallization from EtOAc, m.p. 118°-120°.

후처리

  1. temperatureAfter heating
  2. temperatureto reflux for 2 hrs
  3. distillationthe solvent is distilled off
  4. additionwater is added
  5. temperaturethe mixture refluxed for a further hour
  6. extractionExtraction
  7. customwith methylene chloride and evaporation

출처 및 근거

ORD 기록
ord-648bc41352814c19b6de55e09197bcdd
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05376687

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