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

HRID 1750061ノート

反応式

HRID 1750061 の反応式
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]

参加物

6

反応物 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 1180356092-(2-ethylsulfanyl-4-trifluoromethylsulfanylphenyl)3-methyl-6-pentafluoroethyl-3H-imidazo[4,5-b]pyridine

生成物 1

HCID 1180355032-(2-ethylsulfonyl-4-trifluoromethylsulfanylphenyl)3-methyl-6-pentafluoroethyl-3H-imidazo[4,5-b]pyridine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e34b96037c8f42c0a8246e4a54ac848a
出典データセット
uspto-grants-2015_10
特許番号
US09156838B2

反応ノート

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