Реакция #1435753

ord-0b42858fd1174b349b6ad7db8808e9e5

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe resulting solution was washed with water (3×20 mL)
  2. 2
    Сушкаdried over Na2SO4
  3. 3
    Другоеevaporated to dryness
  4. 4
    workup.DISSOLUTIONThe free base was dissolved in 2-propanol (5 mL)
  5. 5
    ДругоеThe product was crystallized in 2-propanol (5 mL)
  6. 6
    Фильтрацияcollected by filtration, and vacuum
  7. 7
    Другоеdried

Методика

A solution of 3-(6,7-dimethoxy-3,4-dihydro-1H-isoquinolin-2-yl)-propylamine dihydrochloride (323 mg, 1 mmol), N,N-diisopropylethylamine (517 mg, 4 mmol) in CH2Cl2(15 mL), was added 3-Chloro-4,6-difluorobenzenesulfonyl chloride (259 mg, 1.05 mmol) and was stirred overnight at room temperature. The resulting solution was washed with water (3×20 mL) and dried over Na2SO4, and evaporated to dryness. The free base was dissolved in 2-propanol (5 mL). The product was crystallized in 2-propanol (5 mL) collected by filtration, and vacuum dried to give a white solid (401 mg, 87%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07211584B2uspto-grants-2007_05