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

HRID 1052931노트

반응식

HRID 1052931 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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).

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-1722dd911d5d4dd9a6badb63bc404eaf
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09392791B2

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