Reacción #65188

ord-d92df32fa3c24976935b2b186cc36c14

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe organic phase is separated after settling
  2. 2
    Lavadothe solid residue is washed with dichloromethane
  3. 3
    Lavadothe organic phase is washed with a saturated sodium hydrogen carbonate solution
  4. 4
    Secadowith water, it is dried over sodium sulphate
  5. 5
    Otrothe solvent is evaporated under reduced pressure and 22 g of solid
  6. 6
    Otroare obtained
  7. 7
    OtroAfter recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
  8. 8
    Otroare finally obtained

Procedimiento

34 g (0.077 mole) of α-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 500 ml of dichloromethane are treated with 36.9 g (0.24 mole) of Rongalite®, while stirring the mixture at room temperature for 24 h. The organic phase is separated after settling has taken place, the solid residue is washed with dichloromethane, the organic phase is washed with a saturated sodium hydrogen carbonate solution and then with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure and 22 g of solid are obtained. After recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals are finally obtained. Melting point: 194°-195° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05418248uspto-grants-1995_05