Reacción #78158

ord-0ee547c4878842c0b4af4db53c2fdb6f

Condiciones de reacción

Temperatura
90°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    LavadoThe organic phase washed with water
  2. 2
    Secadodried over anhydrous sodium sulfate
  3. 3
    Otrois evaporated
  4. 4
    Otrothe residue purified on silica gel by flash chromatography

Procedimiento

A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.482 g (4.5 mmol) p-toluidine is stirred for 1.5 h at 90° C. under a nitrogen atmosphere. The reaction mixture is then distributed between 30 ml acetate and 20 ml of 20% aqueous potassium carbonate solution. The organic phase washed with water and dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (50:1 to 9:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile and drying under HV; m.p. 152-153° C.; ESI-MS: (M+H)+=327.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06710047B2uspto-grants-2004_03