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Hydrochloric Acid → 2'-Fluoro-2-hydroxy-4-methoxy-3-methylbenzophenone

HRID 568651
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HRID 568651 반응식
C[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:4]=1[CH3:11].[F:12][C:13]1[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15](Cl)=[O:16].[Al+3].[Cl-].[Cl-].[Cl-].Cl>ClC(Cl)C>[F:12][C:13]1[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=1[C:15](=[O:16])[C:8]1[CH:7]=[CH:6][C:5]([O:9][CH3:10])=[C:4]([CH3:11])[C:3]=1[OH:2]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 98082-Fluorobenzoyl chlorideHCID 797552,6-DimethoxytolueneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 130157162'-Fluoro-2-hydroxy-4-methoxy-3-methylbenzophenone

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
5 °C

실험 절차

2,6-dimethoxytoluene (20.0 g) and o-fluorobenzoyl chloride (19.8 g) are dissolved in 250 ml of dichloroethane and chilled to 5° C. AlCl3 is added portiowise and when the addition is complete the reaction mixture is allowed to warm to room temperature over 30 minutes, then refluxed 30 minutes. It is then poured into 5% HCl and allowed to stand undisturbed 18 hours. Extraction with ether, followed by drying and concentration, gives crystalline material that is washed with hexane to give 2'-fluoro-2-hydroxy-4-methoxy-3-methylbenzophenone, mp 118°-120° C.

후처리

  1. additionwhen the addition
  2. temperatureto warm to room temperature over 30 minutes
  3. temperaturerefluxed 30 minutes
  4. extractionExtraction with ether
  5. customby drying
  6. concentrationconcentration
  7. customgives crystalline material that
  8. washis washed with hexane

출처 및 근거

ORD 기록
ord-f624b7e8cba046449b64dcc4643915f7
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04728662

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