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Sulfamide → Tert-butyl 4-sulfamoyl-1,4-diazepane-1-carboxylate

HRID 1175458
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1175458
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[S:15](N)([NH2:18])(=[O:17])=[O:16]>O1CCOCC1>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([S:15](=[O:17])(=[O:16])[NH2:18])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 82267SulfamideHCID 2756058Tert-butyl 1,4-diazepane-1-carboxylate

Produkt 1

HCID 67051265Tert-butyl 4-sulfamoyl-1,4-diazepane-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of 1,4-Diazepane-1-carboxylic acid tert-butyl ester (3.16 g) in dioxane (40 ml) was added sulfamide (4.0 g) and the reaction mixture was then heated at reflux 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: 4.27 g

Aufarbeitung

  1. temperaturethe reaction mixture was then heated
  2. temperatureat reflux for 18 h
  3. customthe residue partitioned between EtOAc (100 ml) and H2O (100 ml)
  4. customThe organics were separated
  5. extractionthe aqueous layer was re-extracted with EtOAc (2×100 ml)
  6. dry with materialdried (MgSO4)

Quellen und Nachweise

ORD-Eintrag
ord-a752dd4f46f541edb532742c00bde94b
Quelldatensatz
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07838675B2

Notizen zur Reaktion

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