Реакция #78149

ord-f2f95fd073184faf8e0ae02848eed4fe

Растворители

Условия реакции

Температура
90°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe organic phase washed with water
  2. 2
    Сушкаdried over sodium sulfate
  3. 3
    Другоеis evaporated
  4. 4
    Другоеthe residue purified on silica gel by flash chromatography

Методика

A mixture of 0.384 g (1.5 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.532 g (4.5 mmol) 4-aminobenzonitrile is heated for 1.5 h at 90° C. The reaction mixture is then distributed between dichloromethane and 20% aqueous potassium carbonate solution. The organic phase washed with water and dried over sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol mixtures (50:1 and). 25:1). Title compound is obtained after crystallization of the product-containing fractions from dichloromethane and drying under HV (8 h, 90° C.); m.p. 228-230° C.; ESI-MS: (M+H)+=338.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06710047B2uspto-grants-2004_03