Реакция #42818

ord-a4af7b81b1104f438edb52c606601f67

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture was cooled to near room temperature
  2. 2
    Экстракцияthe mixture was extracted with tert-butyl methyl ether three times
  3. 3
    ПромывкаThe organic layers were washed with a saturated sodium chloride aqueous solution
  4. 4
    Сушкаdried over anhydrous magnesium sulfate
  5. 5
    Концентрированиеconcentrated

Методика

Into 2 ml of acetonitrile were added 0.20 g of 4-(2-butynyloxy)-6-chloropyrimidine, 0.45 g of potassium carbonate and 0.20 g of 3,3-dimethylpiperidine hydrochloride, and the mixture was stirred for 2 hours at 80° C. The reaction mixture was cooled to near room temperature, a saturated ammonium chloride aqueous solution was added therein, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.27 g of 4-(2-butynyloxy)-6-(3,3-dimethylpiperidino)pyrimidine (hereinafter, referred to as Compound (31)).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07732448B2uspto-grants-2010_06