반응 #711137

ord-d531ce4ecd964391819bc66ded6e5923

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타In a 50-mL round-bottom flask was placed
  2. 2
    농축concentrated under vacuum
  3. 3
    기타The residue was purified by flash column chromatography (silica gel, 100:0-20:1 CH2Cl2:MeOH)

실험 절차

In a 50-mL round-bottom flask was placed a solution of Na (260 mg, 11.3 mmol) in methanol (15 mL) and the solution was stirred for 30 minutes at room temperature. Then 2-chloro-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridine (250 mg, 1.13 mmol, Intermediate 4, step c) was added. The resulting mixture was stirred for 4 hours at 75° C. and concentrated under vacuum. The residue was purified by flash column chromatography (silica gel, 100:0-20:1 CH2Cl2:MeOH) to give the title compound as a light yellow solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09303015B2uspto-grants-2016_04