Реакция #42824

ord-10f01cf55aa34dfcb2edcde7934779c7

Растворители

Условия реакции

Температура
60°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 0.24 g of 3,3,5,5-tetramethylpiperidine hydrochloride, and the mixture was stirred for 4 hours at 60° 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 0.23 g of 4-(2-butynyloxy)-6-(3,3,5,5-tetramethylpiperidino)pyrimidine (hereinafter, referred to as Compound (38)).

Источник

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