Реакция #78145

ord-ac39a0f1f7a347668c01e5f18e9de5ef

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 0.511 g (2 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.576 ml (6 mmol) 4-fluoroaniline is heated for 2 h at 90° C. The residue is then distributed between acetate 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 acetonitrile and drying under HV (6 h, 100° C.); m.p. 129-131° C.; ESI-MS: (M+H)+=331.

Источник

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