Sodium Thiosulfate → 2-(2-ethylsulfonyl-4-trifluoromethylsulfanylphenyl)3-methyl-6-pentafluoroethyl-3H-imidazo[4,5-b]pyridine

HRID 1750061노트

반응식

HRID 1750061 반응식
Cl[C:2]1C=C(C=C[CH:11]=1)C(OO)=O.C(S[C:15]1[CH:20]=[C:19]([S:21][C:22]([F:25])([F:24])[F:23])[CH:18]=[CH:17][C:16]=1[C:26]1[N:41]([CH3:42])[C:29]2=[N:30][CH:31]=[C:32]([C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])[CH:33]=[C:28]2[N:27]=1)C.C(=O)(O)[O-].[Na+].[S:48]([O-:52])([O-])(=[O:50])=S.[Na+].[Na+]>C(Cl)(Cl)Cl>[CH2:2]([S:48]([C:15]1[CH:20]=[C:19]([S:21][C:22]([F:23])([F:25])[F:24])[CH:18]=[CH:17][C:16]=1[C:26]1[N:41]([CH3:42])[C:29]2=[N:30][CH:31]=[C:32]([C:34]([F:40])([F:39])[C:35]([F:36])([F:37])[F:38])[CH:33]=[C:28]2[N:27]=1)(=[O:52])=[O:50])[CH3:11]

참가 물질

6

실험 절차

0.19 g of 3-chloroperoxybenzoic acid (purity of 65% or more) was added to a mixture of 0.19 g of 2-(2-ethylsulfanyl-4-trifluoromethylsulfanylphenyl)3-methyl-6-pentafluoroethyl-3H-imidazo[4,5-b]pyridine and 3 ml of chloroform under ice cooling, and then the mixture was stirred under ice cooling for 2 hours. A saturated aqueous sodium bicarbonate solution and a saturated aqueous sodium thiosulfate solution were added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.22 g of 2-(2-ethylsulfonyl-4-trifluoromethylsulfanylphenyl)3-methyl-6-pentafluoroethyl-3H-imidazo[4,5-b]pyridine (hereinafter, referred to as Compound 10).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e34b96037c8f42c0a8246e4a54ac848a
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09156838B2

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