Реакция #44516

ord-6319f4d90ee340cbb34c2715c3d9de01

Растворители

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияsubjected to extraction with EtOAc
  2. 2
    workup.ADDITIONThen water was added
  3. 3
    Экстракцияthe mixture was subjected to extraction with ethyl acetate
  4. 4
    ПромывкаThe organic layer was washed with water and brine sequentially
  5. 5
    Сушкаdried over anhydrous Na2SO4
  6. 6
    Концентрированиеconcentrated
  7. 7
    ДругоеThe resulting residue was purified by column chromatography

Методика

6-((2-chloropyrimidin-4-yl)(methyl)amino)-N,2-dimethylbenzofuran-3-carboxamide (0.1 mmol) and 3-dimethylaminoaniline (0.1 mmol) were dissolved in 0.5 ml DMF. To this was added p-TsOH monohydrate (0.2 mmol). The reaction mixture was stirred at 60° C. for 5 hours, and subjected to extraction with EtOAc. Then water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with water and brine sequentially, dried over anhydrous Na2SO4, and concentrated. The resulting residue was purified by column chromatography to provide the title product in a yield of 78%.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07737157B2uspto-grants-2010_06