Reaktion #495982

ord-dff0416bf98646839691f01d002b0f15

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to 20° C
  2. 2
    SonstigeThe extracts were separated
  3. 3
    Extraktionthe aqueous layer was extracted with ethyl acetate
  4. 4
    TrocknenThe combined extracts were dried (sodium sulfate)
  5. 5
    Sonstigeevaporated

Vorschrift

2-Ethylpyrazolo[1,5-a]pyridine-3-carboxylic acid (4.1 g, 22 mmol) was stirred in water (100 mL) and sulfuric acid (2.5 mL) was added. The mixture was heated at 70° C. for 2 h and cooled to 20° C. The mixture was poured into ethyl acetate and neutralized with saturated sodium bicarbonate. The extracts were separated and the aqueous layer was extracted with ethyl acetate. The combined extracts were dried (sodium sulfate) and evaporated to give the desired compound (2.6 g, 82%). LCMS for C9H11N2 (M+H)+: m/z=147.1. 1H NMR (300 MHz, DMSO-d6): δ 8.52 (m, 1H), 7.57 (m, 1H), 7.11 (m, 1H), 6.75 (m, 1H), 6.38 (s, 1H), 2.73 (m, 2H), 1.22 (m, 3H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08759359B2uspto-grants-2014_06