Oxygen → 3,5-Octanedione

HRID 132722

반응식

HRID 132722 반응식
O=O.[H-].[Na+].[C:5]([O:10]CC)(=O)[CH2:6][CH2:7][CH3:8].[CH3:13][C:14](=[O:17])[CH2:15][CH3:16]>N#N.O1CCCC1.O>[CH3:16][CH2:15][C:14](=[O:17])[CH2:13][C:5](=[O:10])[CH2:6][CH2:7][CH3:8]

참가 물질

8

반응물 4

HCID 977OxygenHCID 6569Methyl Ethyl KetoneHCID 7762Ethyl butyrateHCID 24758Sodium hydride

생성물 1

HCID 806023,5-Octanedione수율 56.3%

시약·촉매·용매 3

HCID 947Nitrogen용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

In N2 atmosphere free of water and oxygen, to a 3-neck flask placed in an ice-bath and equipped with addition funnel and reflux condenser were successively added 0.07 mol sodium hydride and 100 ml tetrahydrofuran. To the mixture was added dropwise a solution of 0.06 mol ethyl butyrate and 0.03 mol butanone with stirring. Upon completing the addition, the mixture was heated refluxing for 4 hours. The solvent and composition with a boiling point below 110° C. were removed by distillation. To the residue was added an appropriate amount of saturated saline until the solid composition was just dissolved. The mixture was extracted with ethyl ether for three times. The organic phases were combined and dried over anhydrous sodium sulfate. The solvent was removed by distillation to give 2.4 g product.

후처리

  1. customequipped with addition funnel
  2. temperaturereflux condenser
  3. additionthe addition
  4. temperaturethe mixture was heated
  5. temperaturerefluxing for 4 hours
  6. customThe solvent and composition with a boiling point below 110° C. were removed by distillation
  7. additionTo the residue was added an appropriate amount of saturated saline until the solid composition
  8. dissolutionwas just dissolved
  9. extractionThe mixture was extracted with ethyl ether for three times
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was removed by distillation

출처 및 근거

ORD 기록
ord-09f630a0eeb34a17823d5df51424f236
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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