Реакция #45627

ord-b6f53dcdba73465fa9aca3432bd28b74

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураcooled with ice
  2. 2
    workup.STIRRINGstirring at 60° C. for 1 hour
  3. 3
    ТемператураAfter cooling
  4. 4
    Промывкаby washing with water and saturated brine
  5. 5
    СушкаThe obtained organic layer was dried over anhydrous sodium sulfate
  6. 6
    Другоеthe solvent was evaporated away under reduced pressure

Методика

Under nitrogen atmosphere, cinnamoyl chloride (378 mg, 2.27 mmol) was dropwise added to a tetrahydrofuran solution (10 ml) of 2-amino-5-phenyl-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-41) (500 mg, 2.06 mmol) and sodium hydrogencarbonate (399 mg, 4.75 mmol) cooled with ice, followed by stirring at room temperature for 17 hours and stirring at 60° C. for 1 hour. After cooling, ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The obtained organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07737166B2uspto-grants-2010_06