반응 #71474

ord-92c9590d2faa45dc85430e736fa96f66

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux for 72 h
  2. 2
    세척washed with H2O and brine
  3. 3
    건조dried (sodium sulfate)
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    기타The residue was purified by silica gel column chromatography (Hex/EtOAc, 7:3)

실험 절차

Benzyl chloride (1.8 mL, 15.4 mmol, 1.2 equiv) was added to a solution of 2-nitroimidazole (1.45 g, 12.8 mmol) and triethylamine (3.6 mL, 25.7 mmol, 2 equiv) in DCM (40 mL). The reaction mixture was stirred at reflux for 72 h, allowed to cool to rt, diluted with DCM, washed with H2O and brine, dried (sodium sulfate), filtered and concentrated. The residue was purified by silica gel column chromatography (Hex/EtOAc, 7:3) to afford 1.31 g of the title compound as a white solid: ES-MS: 204.0 [M+H]+; tR=3.72 min (System 1); TLC: Rf=0.22 (Hex/EtOAc, 7:3).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536175B2uspto-grants-2013_09