Methanol → HCID 178440154, 화합물

HRID 1249552노트

반응식

HRID 1249552 반응식
[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:25])[F:24])([C:19]([F:22])([F:21])[F:20])[OH:18])[NH:7][C:8]=1[C:9]1[CH:14]=[CH:13][C:12](SC)=[CH:11][CH:10]=1)[CH3:3].O[O:28][S:29]([O-:31])=O.[K+].S(OOS([O-])(=O)=O)(O)(=O)=O.[K+].[CH3:44]O>>[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:24])[F:25])([C:19]([F:20])([F:21])[F:22])[OH:18])[NH:7][C:8]=1[C:9]1[CH:10]=[CH:11][C:12]([S:29]([CH3:44])(=[O:31])=[O:28])=[CH:13][CH:14]=1)[CH3:3]

참가 물질

5

반응물 4

HCID 887MethanolHCID 23690007Potassium hydrogen persulfateHCID 23707502Potassium hydroxy sulfiteHCID 178503127HCID 178503127, 화합물

생성물 1

HCID 178440154HCID 178440154, 화합물

실험 절차

A mixture of 4.0 g (0.01 mole) of 4-(1-methylethyl)-5-(4-methylthiophenyl)-α,α-bis(trifluoromethyl)-1H-imidazole-2-methanol, 16.06 g (0.026 mole) of Oxone® (potassium hydrogen persulfate) and 115 ml of methanol was stirred at room temperature overnight. The inorganic solid was filtered off, and the filtrate was evaporated. The residue was partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water, brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

후처리

  1. filtrationThe inorganic solid was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe layers were separated
  5. washthe organic layer was washed with water, brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

출처 및 근거

ORD 기록
ord-b1c6dbbda2a349a497553983989702f1
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04632930

반응 노트

불러오는 중…