Reacción #9999

ord-d4bf9e65b4ca4dc8a7893f11d1c680e7

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónthe mixture is extracted with water
  2. 2
    SecadoThe organic phase is dried over sodium sulfate
  3. 3
    OtroAfter removal of the solvent
  4. 4
    Otrothe residue is recrystallized from ethyl acetate and diethyl ether

Procedimiento

168 mg (0.5 mmol) of 2-chloro-6-(3,4,5-trimethoxy-phenyl-amino)-purine, 103 mg (0.75 mmol) of potassium carbonate and 0.156 ml (2.5 mmol) of methyl iodide are stirred in 3 ml of dimethylformamide at room temperature for 5 h. 30 ml of ethyl acetate are added to the slightly cloudy reaction solution and the mixture is extracted with water. The organic phase is dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-6-(3,4,5-trimethoxy-phenyl-amino)-9-methyl-9H-purine is obtained; FAB-MS: (M+H)+=350; Rf=0.6 (CH2Cl2:methanol=9:1).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07091346B1uspto-grants-2006_08