Реакция #63890

ord-aea49e6eb2a94a648bb39e9b7a45eb25

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGThis mixture was stirred for 2.5 days
  2. 2
    Экстракцияextracted with 150 ml portions of dichloromethane
  3. 3
    Другоеdried
  4. 4
    Другоеevaporated in vacuo
  5. 5
    ДругоеThe residue was chromatographed

Методика

To 10.0 of N-[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]acetamide in 500 ml of dry dimethylformamide under argon, was added 2.0 g of sodium hydride (50% in oil). This mixture was stirred for 1 hour, then 3.75 ml of 3-bromopropane was added. This mixture was stirred for 2.5 days, then poured into 1 liter of water and extracted with 150 ml portions of dichloromethane. The extracts were combined, dried and evaporated in vacuo. The residue was chromatographed as described in Example 1, giving 3.60 g of the desired product as yellow crystals, mp 145°-149° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04767765uspto-grants-1988_08