Реакция #78173

ord-341da6b698e7474fbf81c9387c641f13

Растворители

Условия реакции

Температура
115°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe cooled reaction mixture
  2. 2
    ПромывкаThe organic solution washed with brine
  3. 3
    Сушкаdried over anhydrous sodium sulfate
  4. 4
    Другоеis evaporated
  5. 5
    Другоеthe residue purified on silica gel by flash chromatography

Методика

A mixture of 0.3 g (1.173 mmol) 1-chloro-4-(4-pyridylmethyl)phthalazine and 0.4 g (4.692 mmol) cyclopentylamine is stirred for 6 h at 115° C. The cooled reaction mixture is then distributed between dichloromethane and saturated aqueous sodium hydrogencarbonate solution. The organic solution washed with brine and dried over anhydrous sodium sulfate is evaporated and the residue purified on silica gel by flash chromatography using acetate/methanol (9:1). Title compound is obtained after crystallization of the product-containing fractions from acetonitrile/water and drying under HV (8 h, 100° C.); m.p. 163-165° C.; ESI-MS: (M+H)+=305.

Источник

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