Реакция #42807

ord-0bf0dadf27e64875acc546a93a5645dc

Растворители

Условия реакции

Температура
120°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added
  2. 2
    ТемператураThe reaction mixture was cooled to near room temperature
  3. 3
    Промывкаthe mixture was washed with a saturated sodium chloride aqueous solution three times
  4. 4
    СушкаThe organic layers were dried over anhydrous magnesium sulfate
  5. 5
    Концентрированиеconcentrated

Методика

Into 2 ml of N,N-dimethylformamide was resolved 183 mg of 4-chloro-6-(2-butynyloxy)pyrimidine, 166 mg of potassium carbonate and 99 mg of 2-methylpiperidine was added therein, and the mixture was stirred for 4 hours at 80 and 3 hours at 120° C. The reaction mixture was cooled to near room temperature, ethyl acetate was added therein, and the mixture was washed with a saturated sodium chloride aqueous solution three times. The organic layers were dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 66 mg of 4-(2-butynyloxy)-6-(2-methylpiperidino)pyrimidine (hereinafter, referred to as Compound (20)).

Источник

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