Реакция #78173
ord-341da6b698e7474fbf81c9387c641f13
Уравнение реакции
Реагенты
Нет
Растворители
Условия реакции
Температура
115°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ДругоеThe cooled reaction mixture
- 2ПромывкаThe organic solution washed with brine
- 3Сушкаdried over anhydrous sodium sulfate
- 4Другоеis evaporated
- 5Другоеthe 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.