Sodium Hydroxide → 2,5-Dimethyl-3-furoic acid

HRID 357793

반응식

HRID 357793 반응식
C([O:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[O:8][C:7]=1[CH3:12])=[O:5])C.[OH-].[Na+]>C(O)C>[CH3:12][C:7]1[O:8][C:9]([CH3:11])=[CH:10][C:6]=1[C:4]([OH:5])=[O:3]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 1414573-Furancarboxylic acid, 2,5-dimethyl-, ethyl ester

생성물 1

HCID 694652,5-Dimethyl-3-furoic acid수율 60%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2,5-Dimethyl-3-furancarboxylic acid ethyl ester (14.6 g) (synthesized in accordance with the method described in J.A.C.S., 59, 2525 (1937)) was dissolved in ethanol (100 15 ml), and 1N aqueous sodium hydroxide (100 ml) was added. The mixture was stirred at room temperature for 1 hour, and then stirred under reflux for 30 minutes. The mixture was concentrated under reduced pressure, and the residue was dissolved in water and washed with diethyl ether. The aqueous layer was acidified with 1N hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. precipitated crystals were recrystallized from acetone-hexane to give 2,5-dimethyl-3-furancarboxylic acid (7.3 g) as crystals.

후처리

  1. stirringstirred
  2. temperatureunder reflux for 30 minutes
  3. concentrationThe mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in water
  5. washwashed with diethyl ether
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with water and saturated aqueous sodium chloride
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customprecipitated crystals
  11. customwere recrystallized from acetone-hexane

출처 및 근거

ORD 기록
ord-47795c4538de4dfa90dae80f48ba7f9c
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840917

연결된 노트

불러오는 중…