Ethanol → Diethyl 2,2-dimethylpentanedioate

HRID 132742

반응식

HRID 132742 반응식
[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8]([OH:10])=[O:9])[C:3]([OH:5])=[O:4].[CH2:12](O)[CH3:13].[C:15]1(C)C=CC=C[CH:16]=1.S(=O)(=O)(O)O>O>[CH3:1][C:2]([CH3:11])([CH2:6][CH2:7][C:8]([O:10][CH2:12][CH3:13])=[O:9])[C:3]([O:5][CH2:15][CH3:16])=[O:4]

참가 물질

6

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 1140TolueneHCID 126812,2-Dimethylglutaric acid

생성물 1

HCID 550221Diethyl 2,2-dimethylpentanedioate수율 90%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 0.1 mol 2,2-dimethyl-glutaric acid were added 0.3 mol ethanol, 40 ml toluene, and 0.4 ml concentrated sulfuric acid with stirring. The mixture was heated refluxing, and the water produced was removed by using a water separator until the amount of the water separated reached theoretical value. The mixture was neutralized with saturated sodium carbonate solution and extracted with ethyl acetate. The upper layer solution was separated, washed with saturated saline until being neutral, and dried over anhydrous sodium sulfate. After the solvent was removed, distillation under reduced pressure gave diethyl 2,2-dimethylglutarate as a colorless liquid, and the yield was 90%.

후처리

  1. temperatureThe mixture was heated
  2. temperaturerefluxing
  3. customwas removed
  4. customseparated
  5. extractionextracted with ethyl acetate
  6. customThe upper layer solution was separated
  7. washwashed with saturated saline
  8. dry with materialdried over anhydrous sodium sulfate
  9. customAfter the solvent was removed
  10. distillationdistillation under reduced pressure

출처 및 근거

ORD 기록
ord-e5342c668a2146d48d412a1ba6d23ca5
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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