2-Bromoethanol → HCID 86629018, Verbindung

HRID 1013437Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1013437
[NH2:1][C@H:2]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:3][C:4]([O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:5].Br[CH2:19][CH2:20][OH:21].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[OH:21][CH2:20][CH2:19][NH:1][C@@H:2]([CH2:3][C:4]([O:6][C:7]([CH3:9])([CH3:10])[CH3:8])=[O:5])[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12]

Komponenten

5

Edukt 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 7269469D-aspartic acid di-t-butyl ester

Produkt 1

HCID 86629018HCID 86629018, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of di-tert-butyl L-aspartate (5.62 g-20 mmol), 2-bromoethanol (2.84 ml-40 mmol) and K2CO3 (5.6 g-40 mmol) in 100 ml of acetonitrile is heated at reflux for 16 hours. The mineral salts are filtered off and the solvent is removed by distillation in vacuo. The crude product so obtained is purified by flash chromatography on silica gel using a (95/5) dichloromethane/ethanol mixture as eluant. The expected product is obtained in the form of a colourless oil.

Aufarbeitung

  1. temperatureat reflux for 16 hours
  2. filtrationThe mineral salts are filtered off
  3. customthe solvent is removed by distillation in vacuo
  4. customThe crude product so obtained
  5. customis purified by flash chromatography on silica gel using a (95/5) dichloromethane/ethanol mixture as eluant

Quellen und Nachweise

ORD-Eintrag
ord-3d01342a0d654d76a4bdc76d6348a218
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07981920B2

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