Reacción #2091

ord-2b41b35df72e44c4adc18e6e041d2837

Condiciones de reacción

Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated at 120° C. for a further 6 hours
  2. 2
    TemperaturaThe reaction mixture was cooled
  3. 3
    FiltraciónThe solid was filtered off with suction
  4. 4
    Lavadowashed with water
  5. 5
    FiltraciónThe crystallizate was filtered
  6. 6
    Lavadowashed with ethanol
  7. 7
    Otrodried under reduced pressure

Procedimiento

16.8 g (0.7 mol) of sodium hydride were introduced in portions with stirring into a suspension of 99.6 g (0.6 mol) of 3-methylxanthine in 1.5 l of dimethylformamide. After evolution of hydrogen had ended, the mixture was heated to 100° C., treated dropwise with 76 g (0.6 mol) of benzyl chloride and heated at 120° C. for a further 6 hours. The reaction mixture was cooled and cautiously poured into 3 l of water. The solid was filtered off with suction and washed with water, the filter residue was taken up in ethanol and the solution was stirred at room temperature for one hour. The crystallizate was filtered, washed with ethanol and dried under reduced pressure.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05728686uspto-grants-1998_03