Реакция #42808

ord-f6e7397cfab14baf90d86a8479bbe747

Растворители

Условия реакции

Температура
60°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 85 mg of 2-methylpyrrolidine was added therein, and the mixture was stirred for 7 hours at 60° 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 207 mg of 4-(2-butynyloxy)-6-(2-methyl-pyrrolidin-1-yl) pyrimidine (hereinafter, referred to as Compound (21)).

Источник

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