Thiosulfate ion → 2-(2-ethylsulfonylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine

HRID 923738노트

반응식

HRID 923738 반응식
C(S[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:22]([CH3:23])[C:13]2=[N:14][CH:15]=[C:16]([C:18]([F:21])([F:20])[F:19])[CH:17]=[C:12]2[N:11]=1)C.Cl[C:25]1C=CC=C(C(OO)=O)[CH:26]=1.[Na].[S:36]([O-:40])([O-])(=[O:38])=S>C(Cl)(Cl)Cl>[CH2:25]([S:36]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10]1[N:22]([CH3:23])[C:13]2=[N:14][CH:15]=[C:16]([C:18]([F:21])([F:19])[F:20])[CH:17]=[C:12]2[N:11]=1)(=[O:40])=[O:38])[CH3:26]

참가 물질

6

반응물 4

HCID 1084Thiosulfate ionHCID 70297m-Chloroperbenzoic acidHCID 5360545SodiumHCID 867081912-(2-ethylsulfanylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine

생성물 1

HCID 867081932-(2-ethylsulfonylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a mixture of 2-(2-ethylsulfanylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (0.25 g) and chloroform (3 ml), 3-chloroperbenzoic acid (purity: not less than 65%, 0.43 g) was added under ice-cooling, and then heated to room temperature, and stirred for 1 hour. To the reaction mixture, chloroform was added under ice-cooling, and then saturated aqueous sodium, thiosulfate solution was poured, and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution, then saturated trine, dried over sodium sulfate, and concentrated under reduced pressure. The obtained crystal was washed with hexane, then methyl-tert-butyl ether to give 0.27 g of 2-(2-ethylsulfonylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (hereinafter referred to as Present Compound 6).

후처리

  1. additionwas added under ice-
  2. temperaturecooling
  3. temperaturecooling
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution
  6. dry with materialsaturated trine, dried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. washThe obtained crystal was washed with hexane

출처 및 근거

ORD 기록
ord-7baa4351a19b47b28a643401a0a0ddbb
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278983B2

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