Reaktion #1363058

ord-4362875e2d8d4b4fbdb89a614c12f7c4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 20 hours
  2. 2
    TemperaturAfter cooling
  3. 3
    Waschenthe reaction mixture was washed with saturated aqueous sodium bicarbonate
  4. 4
    Trocknendried (MgSO4)
  5. 5
    Sonstigeevaporated under reduced pressure
  6. 6
    SonstigePurification
  7. 7
    Wascheneluting with 40% ethyl acetate in isohexane

Vorschrift

2-Methyl-4-thiazolecarboxylic acid ethyl ester (1 g) (Liebigs Ann. Chem. 1981, 623), N-bromosuccinimide (1.04 g) and a catalytic amount of benzoyl peroxide in chloroform (25 ml) was heated at reflux for 20 hours. After cooling, the reaction mixture was washed with saturated aqueous sodium bicarbonate, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 40% ethyl acetate in isohexane to give the product as an oil. Yield 0.5 g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06162808uspto-grants-2000_12