Oxygen → 3,5-Octanedione

HRID 132722

反応式

HRID 132722 の反応式
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]

参加物

8

反応物 4

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

生成物 1

HCID 806023,5-Octanedione収率 56.3%

試薬・触媒・溶媒 3

HCID 947Nitrogen溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09f630a0eeb34a17823d5df51424f236
出典データセット
uspto-grants-2008_06
特許番号
US07388061B2

関連ノート

読み込み中…