반응 #522324

ord-cb758bfd24dc44a2888cc0a9287c694b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The resulting solution was heated
  2. 2
    온도to reflux temperature
  3. 3
    온도The solution was cooled
  4. 4
    추출The resulting composition was extracted with 200 ml of ether
  5. 5
    세척The ether phase was then sequentially washed with 100 ml of water
  6. 6
    건조The ether phase was dried over magnesium sulfate
  7. 7
    여과filtered
  8. 8
    농축concentrated
  9. 9
    기타a rotary evaporator

실험 절차

Approximately 18.1 g of 4-methyl-3-nitrobenzoic acid was added to approximately 50 ml of methanol. Approximately 2 ml of concentrated sulfuric acid was added to this solution. The resulting solution was heated to reflux temperature and stirred at this temperature for 16 hours. The solution was cooled and approximately 300 ml of water was added. The resulting composition was extracted with 200 ml of ether. The ether phase was saved and the aqueous phase was discarded. The ether phase was then sequentially washed with 100 ml of water, followed by 100 ml of 10% aqueous sodium carbonate. The ether phase was dried over magnesium sulfate, filtered, and concentrated using a rotary evaporator and a water aspirator vacuum to yield 17.3 g of 4-methoxycarbonyl-2-nitrotoluene as a viscous oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04400461uspto-grants-1983_08