반응 #91961

ord-fd7d3d0d52534756aaac68f7b89eb398

용매

반응 조건

온도
35°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도refluxed for 2 h
  2. 2
    기타The solvent was removed
  3. 3
    기타the residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%)
  4. 4
    기타to afford brown solid AB (587 mg, 67%)

실험 절차

To a solution of 5-methyloxazole-4-carbonitrile AA (0.76 g, 7.0 mmol) in anhydrous MeOH (30 mL) was added MeONa (0.57 g, 10 mmol), after stirred at 35° C. under nitrogen for 3 h, NH4Cl (0.75 g, 14 mmol) was added, refluxed for 2 h. The solvent was removed and the residue was purified by flash chromatography (Biotage, 40 g silica gel, MeOH in DCM 5%˜35%) to afford brown solid AB (587 mg, 67%). 1H NMR (DMSO-d6, 400 MHz) δ ppm: 9.11-9.19 (m, 3H), 8.60 (s, 1H), 2.59 (s, 3H). MS: calc'd (MH+) 126, measured (MH+) 126.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447086B2uspto-grants-2016_09