tert-Butylacrylamide → HCID 14297377, Verbindung

HRID 845883

Reaktionsgleichung

Reaktionsgleichung von HRID 845883
[CH2:1]([N:8]([CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[OH:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].[C:23]([NH:27][C:28](=[O:31])[CH:29]=[CH2:30])([CH3:26])([CH3:25])[CH3:24]>O1CCCC1>[C:23]([NH:27][C:28](=[O:31])[CH2:29][CH2:30][O:9][N:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)([CH3:26])([CH3:25])[CH3:24]

Komponenten

5

Edukt 3

HCID 7877tert-ButylacrylamideHCID 69297DibenzylhydroxylamineHCID 23665647Potassium tert-butoxide

Produkt 1

HCID 14297377HCID 14297377, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 21.33 g of dibenzylhydroxylamine in 100 ml of dry tetrahydrofuran is admixed with 1.12 g of potassium-tert-butoxide followed by 12.70 g of N-tert-butylacrylamide. The solution is heated under reflux for 24 hours under N2. The crude reaction mixture is concentrated under reduced pressure and the residue is partitioned between water and methylene chloride. The organic layer is washed with water, brine dried (MgSO4) and evaporated under reduced pressure. Purification by liquid chromatography affords the title compound as an oil.

Aufarbeitung

  1. temperatureThe solution is heated
  2. temperatureunder reflux for 24 hours under N2
  3. customThe crude reaction mixture
  4. concentrationis concentrated under reduced pressure
  5. customthe residue is partitioned between water and methylene chloride
  6. washThe organic layer is washed with water, brine
  7. dry with materialdried (MgSO4)
  8. customevaporated under reduced pressure
  9. customPurification by liquid chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ae0ad8f5f7034c5786f95eee030825cc
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04760179

Verknüpfte Notizen

Wird geladen…