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Oxygen → 3-ethyl-2,4-pentanediol Dibenzoate

HRID 132720
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 132720
O=O.[CH2:3]([CH:5]([CH:9]([OH:11])[CH3:10])[CH:6]([OH:8])[CH3:7])[CH3:4].N1C=C[CH:15]=[CH:14][CH:13]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[CH2:27]1[CH2:31][O:30][CH2:29][CH2:28]1>N#N.O>[C:18]([O:8][CH:6]([CH:5]([CH2:3][CH3:4])[CH:9]([O:11][C:29](=[O:30])[C:28]1[CH:27]=[CH:31][CH:15]=[CH:14][CH:13]=1)[CH3:10])[CH3:7])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 977OxygenHCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 218678653-Ethyl-2,4-pentanediol

Produkt 1

HCID 231259023-ethyl-2,4-pentanediol Dibenzoate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 947
Nitrogen
Lösungsmittel
HCID 962WaterLösungsmittel

Versuchsvorschrift

In N2 atmosphere free of water and oxygen, to a reactor were successively added 0.02 mol 3-ethyl-2,4-pentanediol, 20 ml THF, and 0.06 mol pyridine, then slowly added dropwise 0.05 mol benzoyl chloride. The reaction was heated refluxing for 8 hours, and allowed to continue at room temperature for further 12 hours. After the reaction was finished, the reaction mixture was filtered and the cake was washed with anhydrous ethyl ether for three times. The organic phase was completely washed with saturated saline, and dried over anhydrous sodium sulfate. Removing the solvent gave 5.1 g product.

Aufarbeitung

  1. temperatureThe reaction was heated
  2. temperaturerefluxing for 8 hours
  3. filtrationthe reaction mixture was filtered
  4. washthe cake was washed with anhydrous ethyl ether for three times
  5. washThe organic phase was completely washed with saturated saline
  6. dry with materialdried over anhydrous sodium sulfate
  7. customRemoving the solvent

Quellen und Nachweise

ORD-Eintrag
ord-8f2f5528e6f94937a17744271aec00d2
Quelldatensatz
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07388061B2

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