Methanol → HCID 178440127, 화합물

HRID 1249554노트

반응식

HRID 1249554 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])[NH2:18])[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])[NH2:18])[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 178503126HCID 178503126, 화합물

생성물 1

HCID 178440127HCID 178440127, 화합물

실험 절차

A mixture of 1.8 g (4.5 mmoles) of 4-(1-methylethyl)-5-(4-methylthiophenyl)-α,α-bis(trifluoromethyl)-1H-imidazole-2-methanamine, 7.25 g (11.8 mmoles) of Oxone® (potassium hydrogen persulfate) and 50 ml of methanol were stirred together overnight. The solid was filtered off and the filtrate was evaporated in vacuo. The residue was partitioned between ethyl acetate and water and the layers were separated. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford 2.1 g of an oil. The product was purified via flash chromatography on silica gel (73:27 hexane/ethyl acetate) to afford 1.02 g (53%) of the title compound as an off-white crystalline solid, m.p. 155°-157° C.

후처리

  1. filtrationThe solid was filtered off
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was partitioned between ethyl acetate and water
  4. customthe layers were separated
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2ddad78127a04d1fa487356fe01948d8
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04632930

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