Sodium Thiosulfate → N-ethyl-2-ethylsulfonyl-4-trifluoromethyl-N-(5-trifluoromethyl-pyridin-2-yl)-benzamide

HRID 1052931ノート

反応式

HRID 1052931 の反応式
Cl[C:2]1C=CC=C(C(OO)=O)[CH:3]=1.[CH2:12]([N:14]([C:30]1[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][N:31]=1)[C:15](=[O:29])[C:16]1[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][C:17]=1SCC)[CH3:13].C(=O)(O)[O-].[Na+].[S:45]([O-:49])([O-])(=[O:47])=S.[Na+].[Na+]>C(Cl)(Cl)Cl>[CH2:12]([N:14]([C:30]1[CH:35]=[CH:34][C:33]([C:36]([F:38])([F:37])[F:39])=[CH:32][N:31]=1)[C:15](=[O:29])[C:16]1[CH:17]=[CH:18][C:19]([C:22]([F:23])([F:24])[F:25])=[CH:20][C:21]=1[S:45]([CH2:2][CH3:3])(=[O:49])=[O:47])[CH3:13]

参加物

6

反応物 4

HCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 118035603N-ethyl-2-ethylsulfanyl-4-trifluoromethyl-N-(5-trifluoromethyl-pyridin-2-yl)-benzamide

生成物 1

HCID 72944739N-ethyl-2-ethylsulfonyl-4-trifluoromethyl-N-(5-trifluoromethyl-pyridin-2-yl)-benzamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

0.27 g of m-chloroperbenzoic acid (purity of 68%) was added to a mixture of 0.20 g of N-ethyl-2-ethylsulfanyl-4-trifluoromethyl-N-(5-trifluoromethyl-pyridin-2-yl)-benzamide and 5 mL of chloroform under ice cooling, and the mixture was stirred at room temperature for 3 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 concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.26 g of N-ethyl-2-ethylsulfonyl-4-trifluoromethyl-N-(5-trifluoromethyl-pyridin-2-yl)-benzamide (hereinafter, referred to as Compound of Present Invention 5).

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-1722dd911d5d4dd9a6badb63bc404eaf
出典データセット
uspto-grants-2016_07
特許番号
US09392791B2

反応ノート

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