Reaktion #88771

ord-e2250f4e4a344f9993fe2ef6189dd0dd

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to RT
  2. 2
    Filtrationfiltered
  3. 3
    EinengenThe filtrate was concentrated
  4. 4
    Sonstigedried to a residue which
  5. 5
    Sonstigewas purified by Prep TLC
  6. 6
    Wascheneluted with PE/EA (2:1)

Vorschrift

To a solution of 5-(1-hydroxy-3-methylbutyl)-6-isopropoxy-1-methyl-3-(3-(tetrahydro-2H-pyran-2-yloxy)propyl)pyrido[2,3-d]pyrimidine-2,4(1H,3H)-dione (60 mg, 0.13 mmol) in HCOOH (2 mL) was added Zn dust (42 mg, 0.65 mmol). The reaction was heated at 80° C. for 1 h, cooled to RT and filtered. The filtrate was concentrated and dried to a residue which was purified by Prep TLC eluted with PE/EA (2:1) to give 3-(5-isopentyl-6-isopropoxy-1-methyl-2,4-dioxo-1,2-dihydropyrido[2,3-d]pyrimidin-3(4H)-yl)propyl formate (48 mg, 82.7% yield) as a white solid. LCMS: MH+ 392 and TR=2.964 min.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440972B2uspto-grants-2016_09