반응 #1565873

ord-31107afb92b8436d83aa89d360b7bbc9

용매

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to 20° C
  2. 2
    기타The extracts were separated
  3. 3
    추출the aqueous layer was extracted with ethyl acetate
  4. 4
    건조The combined extracts were dried (sodium sulfate)
  5. 5
    기타evaporated

실험 절차

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, 1 H), 7.57 (m, 1 H), 7.11 (m, 1 H), 6.75 (m, 1 H), 6.38 (s, 1 H), 2.73 (m, 2 H), 1.22 (m, 3 H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09403847B2uspto-grants-2016_08