Reaktion #1132856

ord-f8f3e04793db47c2ad9eac4b63976e5b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux for 18 hours
  2. 2
    Sonstigewas removed under reduced pressure
  3. 3
    Filtrationthe resulting solid was filtered
  4. 4
    Waschenwashed with water
  5. 5
    Sonstigedried

Vorschrift

A solution of 3-oxo-3-(2-phenyl-pyrimidin-4-yl)-propionic acid ethyl ester (2.74 g, 10.1 mmol), N-methylthiourea (1.39 g, 15.5 mmol) and 1,8-diazabicyclo[5,4,0]undec-7-en (1.57 g, 10.3 mmol) in ethanol (30 ml) was heated under reflux for 18 hours. After the solution was acidified by addition of hydrochloric acid, ethanol was removed under reduced pressure, and the resulting solid was filtered, washed with water and dried to afford 2-mercapto-1-methyl-2′-phenyl-1H-[4,4′]bipyrimidinyl-6-one (2.78 g, 93%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08569294B2uspto-grants-2013_10