Chlorosulfamic acid → HCID 66747382, Verbindung

HRID 471557Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 471557
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH:11]([CH3:13])[CH3:12])[C:3]=1[C:4]#[N:5].[S:14](Cl)(=[O:17])(=[O:16])[NH2:15]>CC(N(C)C)=O.O>[S:14]([NH2:1])([NH2:15])(=[O:17])=[O:16].[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH:11]([CH3:13])[CH3:12])[C:3]=1[C:4]#[N:5]

Komponenten

5

Edukt 2

HCID 24499Chlorosulfamic acidHCID 66745948HCID 66745948, Verbindung

Produkt 1

HCID 66747382HCID 66747382, VerbindungAusbeute 191,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

To a solution of 2-amino-6-(isopropylamino)benzonitrile (Example 90b) (0.09 g, 0.54 mmol) in DMA (3 mL) was added sulfamoyl chloride (0.19 g, 1.62 mmol). The reaction mixture was stirred at room temperature under nitrogen for 2 hours, diluted with H2O (5 mL) and extracted with EtOAc. Solvents of the combined organic phases were evaporated and the residue was purified by preparative thin layer chromatography using a Hexane/EtOAc (3:2) solution as eluant, to give 2-amino-6-(isopropylamino)benzonitrile sulfamide (0.14 g). MS 255 (MH+).

Aufarbeitung

  1. extractionextracted with EtOAc
  2. customSolvents of the combined organic phases were evaporated
  3. customthe residue was purified by preparative thin layer chromatography

Quellen und Nachweise

ORD-Eintrag
ord-18b3d31e373144209e6050baf94784d0
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08633186B2

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