Potassium Iodide → 1-(2-(Benzyloxy)-4-fluorophenyl)ethanone

HRID 579794

반응식

HRID 579794 반응식
C(N1CCC(CN[C:12]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2F)=[S:13])CC1)(=O)C.[F:22][C:23]1[CH:28]=[CH:27][C:26]([C:29](=[O:31])[CH3:30])=[C:25]([OH:32])[CH:24]=1.Cl[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1.C(=O)([O-])[O-:42].[K+].[K+].[I-].[K+]>CC(=O)C>[N:14]([C:15]1[CH:16]=[CH:17][C:18]2[O:42][CH2:30][CH2:29][O:31][C:19]=2[CH:20]=1)=[C:12]=[S:13].[F:22][C:23]1[CH:28]=[CH:27][C:26]([C:29](=[O:31])[CH3:30])=[C:25]([O:32][CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH:24]=1

참가 물질

8

반응물 5

HCID 4875Potassium IodideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 27373264'-Fluoro-2'-hydroxyacetophenoneHCID 21241609N-[(1-acetyl-4-piperidinyl)methyl]-N'-(2-fluorophenyl)thiourea

생성물 2

HCID 27761732,3-Dihydro-1,4-benzodioxin-6-yl isothiocyanateHCID 212415771-(2-(Benzyloxy)-4-fluorophenyl)ethanone수율 58%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 13 parts of 1-(4-fluoro-2-hydroxyphenyl)ethanone, 14.9 parts of (chloromethyl)benzene, 16.4 parts of potassium carbonate, 0.1 parts of potassium iodide and 120 parts of 2-propanone was stirred overnight at reflux temperature. The reaction mixture was evaporated. The reaction mixture was poured into water. The product was extracted three times with trichloromethane. The combined extracts were dried, filtered and evaporated. The residue was crystallized from a mixture of 2-propanol and water. The product was filtered off and dried, yielding 11 parts (58%) of 1-[4-fluoro-2-(phenylmethoxy)phenyl]ethanone (intermediate 76).

후처리

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. additionThe reaction mixture was poured into water
  4. extractionThe product was extracted three times with trichloromethane
  5. customThe combined extracts were dried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was crystallized from a mixture of 2-propanol and water
  9. filtrationThe product was filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-999acce87e7e48318b5901a2eb848d87
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04749702

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