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Hydrochloric Acid → HCID 87462564, 화합물

HRID 534693
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HRID 534693 반응식
[C:1]1([S:7][C:8]([S:11](F)(=[O:13])=[O:12])([F:10])[F:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:15]([NH2:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.Cl>ClCCCl>[CH2:15]([NH:22][S:11]([C:8]([F:10])([F:9])[S:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:13])=[O:12])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 23726265HCID 23726265, 화합물2회

생성물 1

HCID 87462564HCID 87462564, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

Added to a solution of 1,2-dichloroethane (15 ml), containing the PhSCF2SO2F (1.46 g, 5 mmol) obtained according to the method from example 7, was freshly distilled benzylamine (2.7 ml, 25 mmol). The mixture was stirred and heated at 50° C. for 20 h until the disappearance of PhSCF2SO2F (monitored by TLC and 19F NMR/CDCl3). After returning to ambient temperature, an aqueous solution of HCl (10%) was added to the reaction medium. The aqueous and organic phases were separated and the aqueous phase was extracted with dichloromethane. The organic phases were combined and dried over MgSO4. After filtration and evaporation of the solvents, the residue was purified by chromatography over silica gel (pentane to pentane/AcOEt:4/1). The sulfonamide product was obtained in the form of a white solid (1.5 g, 90%).

후처리

  1. customobtained
  2. customAfter returning to ambient temperature
  3. customThe aqueous and organic phases were separated
  4. extractionthe aqueous phase was extracted with dichloromethane
  5. dry with materialdried over MgSO4
  6. filtrationAfter filtration and evaporation of the solvents
  7. customthe residue was purified by chromatography over silica gel (pentane to pentane/AcOEt:4/1)

출처 및 근거

ORD 기록
ord-33364c33f978447a95ccffb5ee2ccdd5
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853448B2

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