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Hydrochloric Acid → HCID 87462564、化合物

HRID 534693
ノート
印刷プレビュー

反応式

HRID 534693 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7504BenzylamineHCID 23726265HCID 23726265、化合物2 回

生成物 1

HCID 87462564HCID 87462564、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-33364c33f978447a95ccffb5ee2ccdd5
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853448B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート