Acetic Anhydride → HCID 10968127, Verbindung

HRID 1899768

Reaktionsgleichung

Reaktionsgleichung von HRID 1899768
[CH3:1][CH:2]([CH2:4][C@H:5]([NH2:17])[C:6]([NH:8][C@H:9]([C:14]([OH:16])=[O:15])[CH2:10][CH:11]([CH3:13])[CH3:12])=[O:7])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[C:24](OC(=O)C)(=[O:26])[CH3:25]>O.CCOCC>[NH:17]([C:24]([CH3:25])=[O:26])[C@H:5]([C:6]([NH:8][C@H:9]([C:14]([OH:16])=[O:15])[CH2:10][CH:11]([CH3:12])[CH3:13])=[O:7])[CH2:4][CH:2]([CH3:1])[CH3:3]

Komponenten

6

Edukt 3

HCID 7918Acetic AnhydrideHCID 11430Potassium CarbonateHCID 76807L-leucyl-L-leucine

Produkt 1

HCID 10968127HCID 10968127, VerbindungAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

Leu-Leu (1.0 g, 3.8 mmol) and potassium carbonate (7.0 g, 5 mmol) are dissolved in 100 ml of water. The solution is cooled with ice and 5.0 ml acetic anhydride in 50 ml of ether is added dropwise under vigorous stirring. Stirring is continued for one hour, then the ice-bath is removed and the stirring continued for further 2 hours. The water phase is separated, acidified with hydrochloric acid. The precipitate is stirred for one hour, filtered, washed with water and dried yielding 0.8 gram (74%) of Ac-Leu-Leu.

Aufarbeitung

  1. additionis added dropwise under vigorous stirring
  2. customthe ice-bath is removed
  3. waitthe stirring continued for further 2 hours
  4. customThe water phase is separated
  5. stirringThe precipitate is stirred for one hour
  6. filtrationfiltered
  7. washwashed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-6ebe60014d404a9ca117188e58594aef
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05574014

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