Carbon Dioxide → 5-Ethylfuran-2-carboxylic acid

HRID 357784

반응식

HRID 357784 반응식
[CH2:1]([C:3]1[O:4][CH:5]=[CH:6][CH:7]=1)[CH3:2].C([Li])CCC.[C:13](=[O:15])=[O:14].Cl>C(OCC)C>[CH2:1]([C:3]1[O:4][C:5]([C:13]([OH:15])=[O:14])=[CH:6][CH:7]=1)[CH3:2]

참가 물질

6

반응 조건

온도
-70 °C

실험 절차

2-Ethylfuran (9.1 g) was dissolved in diethyl ether, and the mixture was cooled to -70° C. under nitrogen atmosphere. n-Butyllithium (1.6M in hexane, 60 ml) was slowly added dropwise. The mixture was stirred at room temperature for 2 hours, and then cooled to -70° C. The mixture was stirred for 30 minutes with introducing carbon dioxide gas, and then warmed to room temperature. The mixture was stirred at room temperature for 30 minutes, poured into ice-water, acidified with concentrated hydrochloric acid and extracted with diethyl ether. The extract was washed with saturated aqueous sodium chloride and concentrated under reduced pressure. The residue was crystallized from water and collected by filtration to give 5-ethyl-2-furancarboxylic acid (9.0 g).

후처리

  1. temperaturecooled to -70° C
  2. temperaturewarmed to room temperature
  3. stirringThe mixture was stirred at room temperature for 30 minutes
  4. extractionextracted with diethyl ether
  5. washThe extract was washed with saturated aqueous sodium chloride
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was crystallized from water
  8. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-e00fc9bcc5b445959acaa706c66bdc95
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840917

연결된 노트

불러오는 중…