1-Methylpiperazine → 4-Methylpiperazine-1-sulfonamide

HRID 1024950Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1024950
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[S:8](N)([NH2:11])(=[O:10])=[O:9]>O1CCOCC1>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:8]([NH2:11])(=[O:10])=[O:9])[CH2:4][CH2:3]1

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 82267Sulfamide

Produkt 1

HCID 143260054-Methylpiperazine-1-sulfonamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

To a solution of 1-Methylpiperazine (1.58 g) in dioxane was added sulfamide (4.0 g) and the reaction mixture was then heated at reflux in dioxane for 18 h. The reaction mixture was then reduced in vacuo and the residue partitioned between EtOAc (100 ml) and H2O (100 ml). The organics were separated and the aqueous layer was re-extracted with EtOAc (2×100 ml). Organics were combined, dried (MgSO4) and reduced in vacuo to give the subtitle compound as a white solid. Yield: 640 mg

Aufarbeitung

  1. temperaturethe reaction mixture was then heated
  2. customthe residue partitioned between EtOAc (100 ml) and H2O (100 ml)
  3. customThe organics were separated
  4. extractionthe aqueous layer was re-extracted with EtOAc (2×100 ml)
  5. dry with materialdried (MgSO4)

Quellen und Nachweise

ORD-Eintrag
ord-cba9df925b294b0e85a998349db0ce7e
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08722883B2

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