Reaktion #65187

ord-913f9c7fd66746ae845bdb59c546d7cd

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONis added
  2. 2
    SonstigeThe solvent is evaporated under reduced pressure
  3. 3
    Filtrationthe compound is collected by filtration, it
  4. 4
    Waschenis washed with water up to neutral pH
  5. 5
    Sonstigewith ethanol and finally with ethyl ether and it is purified by recrystallization from methanol

Vorschrift

1.6 g (0.005 mole) of 2-(5-methylthien-2-yl)imidazo[2,1-b]-benzothiazole-3-acetic acid are treated, at room temperature, with 0.85 g (0.005 mole) of N,N'-carbonyldiimidazole in 30 ml of anhydrous tetrahydrofuran for 3 h 30 min. A solution composed of 3 g (0.05 mole) of propylamine in 10 ml of anhydrous tetrahydrofuran is added and the mixture is stirred for 4 h at room temperature. The solvent is evaporated under reduced pressure, the compound is collected by filtration, it is washed with water up to neutral pH, then with ethanol and finally with ethyl ether and it is purified by recrystallization from methanol. 1.1 g of a light yellow solid are obtained. Melting point: 204°-206° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05418248uspto-grants-1995_05