Реакция #1002924

ord-d4f40c2eb7f745509f9fcd77489c0491

Растворители

Условия реакции

Температура
100°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONare added
  2. 2
    workup.ADDITIONThe reaction mixture is introduced into a sealed autoclave
  3. 3
    ТемператураAfter cooling
  4. 4
    Другоеthe solvent is evaporated off under reduced pressure
  5. 5
    ФильтрацияThe insoluble material is collected by filtration
  6. 6
    Промывкаwashed with water
  7. 7
    Другоеdried
  8. 8
    ДругоеThe precipitate is then recrystallised from a minimum of ethyl acetate with the aid
  9. 9
    Температураof heat
  10. 10
    ТемператураAfter cooling
  11. 11
    Фильтрацияthe title compound is collected by filtration
  12. 12
    Промывкаwashed with a minimum of ethyl acetate
  13. 13
    Другоеdried

Методика

150 mg of the compound obtained in Step A of Example 1 are dissolved in 8 ml of acetonitrile, to which 300 mg of K2CO3 and 0.15 ml of 1-bromo-4-fluorobutane are added. The reaction mixture is introduced into a sealed autoclave and is heated at 100° C. for 3 hours. After cooling, the solvent is evaporated off under reduced pressure and the residue is taken up in a minimum of water. The insoluble material is collected by filtration, washed with water and dried. The precipitate is then recrystallised from a minimum of ethyl acetate with the aid of heat. After cooling, the title compound is collected by filtration, washed with a minimum of ethyl acetate and dried.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07268129B2uspto-grants-2007_09