반응 #88078

ord-821743cb204d42a1a8a745aa8aed2a07

용매

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to room temperature
  2. 2
    기타partitioned between ethyl acetate and brine
  3. 3
    기타The organic layer was separated
  4. 4
    건조dried over MgSO4
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure

실험 절차

To a solution of 3-iodo-4-methyl-5-nitro-benzoic acid (16.06 g, 52.3 mmol) in acetone (300 mL) was added K2CO3 (14.46 g, 104.6 mmol) followed by methyl iodide ((3.91 mL, 62.76 mmol). The reaction mixture was stirred at 40° C. overnight, then cooled to room temperature and partitioned between ethyl acetate and brine. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to provide 16.5 g (98%) of 3-iodo-4-methyl-5-nitro-benzoic acid methyl ester.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09440956B2uspto-grants-2016_09