반응 #63890

ord-aea49e6eb2a94a648bb39e9b7a45eb25

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThis mixture was stirred for 2.5 days
  2. 2
    추출extracted with 150 ml portions of dichloromethane
  3. 3
    기타dried
  4. 4
    기타evaporated in vacuo
  5. 5
    기타The residue was chromatographed

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04767765uspto-grants-1988_08