Реакция #489703

ord-443867873dda4ba49a649b54c0bc50c0

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураAfter cooling down to room temperature
  2. 2
    Фильтрацияthe reaction mixture was filtered
  3. 3
    Другоеthe filtrate was evaporated
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  5. 5
    Промывкаwashed with water
  6. 6
    Сушкаdried with magnesium sulfate
  7. 7
    Другоеevaporated
  8. 8
    ДругоеFinal purification by preparative HPLC

Методика

14.74 g (74.6 mmol) of 7-chloro-6-fluoro-2H-isoquinolin-1-one (7) were dissolved in 150 ml of toluene. After addition of 30.86 g (111.9 mmol) of silver carbonate and 15.31 g (89.5 mmol) of benzyl bromide, the mixture was stirred at 80° C. for 3 h. After cooling down to room temperature, the reaction mixture was filtered and the filtrate was evaporated. The residue was dissolved in dichloromethane and washed with water, dried with magnesium sulfate and evaporated. Final purification by preparative HPLC gave 11.63 g of the title compound. Rt=2.51 min (Method B). Detected mass: 288.1/290.1 (M+H+).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08742116B2uspto-grants-2014_06