Reacción #70946

ord-455a05bf8ee44cd499497054cc30d7a4

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Lavadowashed with water
  2. 2
    SecadoThe organic phase was dried over anhydrous magnesium sulphate
  3. 3
    Filtraciónfiltered
  4. 4
    Otroevaporated to dryness
  5. 5
    Otroto leave a crude residue that
  6. 6
    Otrowas recrystallised from a dichloromethane/isopropanol mixture

Procedimiento

To a stirred solution of 3,4-dimethoxy-5-nitro-benzoyl chloride (0.50 g, 2.04 mmol) in dichloromethane (10 mL) at 0° C., was added dropwise methylamine (1.02 mL, 2.04 mmol, 2 M in THF). The reaction mixture was stirred at room temperature till all starting material disappeared, then diluted with dichloromethane and washed with water. The organic phase was dried over anhydrous magnesium sulphate, filtered and evaporated to dryness to leave a crude residue that was recrystallised from a dichloromethane/isopropanol mixture to afford 3,4-dimethoxy-N-methyl-5-nitro-benzamide, 0.44 g (89%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08536203B2uspto-grants-2013_09