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Acetic Anhydride → HCID 20465612, Verbindung

HRID 435797
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 435797
[OH:1][CH2:2][CH2:3]CCCC1CCCC1=O.OCCCCCC1CCCC1=O.[C:25]([O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH:34]1[CH2:38][CH2:37][CH2:36][C:35]1=[O:39])(=[O:27])[CH3:26].O.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(OC(=O)C)(=O)C>>[C:2]([O:39][C:35]1[CH2:36][CH2:37][CH2:38][C:34]=1[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][O:28][C:25](=[O:27])[CH3:26])(=[O:1])[CH3:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 7918Acetic Anhydride2×HCID 521998p-Toluenesulfonic acid monohydrateHCID 204655182-(5-Hydroxypentyl)cyclopentan-1-oneHCID 867329372-(5-Hydroxypentyl)cyclopentanone 2-(5-acetoxypentyl)-cyclopentanone

Produkt 1

HCID 20465612HCID 20465612, Verbindung

Versuchsvorschrift

A solution of 400 g. (2.04 moles) of a mixture of 2-(5-hydroxypentyl)cyclopentanone and 2-(5-acetoxypentyl(cyclopentanone (Example 49) and 4.0 g. of p-toluenesulfonic acid monohydrate in 1 l. of acetic anhydride is refluxed at a rate to maintain a steady distillation of acetic acid from the reaction through a helice-packed fractionation column. The reaction is continued with the addition of acetic anhydride to maintain a constant volume until complete conversion of starting materials to product is evident. The mixture is cooled and partitioned between 2 l. of hexane and 3 l. of cold water containing solid sodium bicarbonate to maintain a neutral pH. The organic phase is washed with saturated brine, dried (MgSO4), and evaporated to yield 452 g. of an oil.

Aufarbeitung

  1. temperatureto maintain
  2. distillationa steady distillation of acetic acid
  3. customfrom the reaction through a helice-packed fractionation column
  4. temperatureto maintain a constant volume until complete conversion of starting materials to product
  5. temperatureThe mixture is cooled
  6. custompartitioned between 2 l
  7. temperatureof cold water containing solid sodium bicarbonate to maintain a neutral pH
  8. washThe organic phase is washed with saturated brine
  9. dry with materialdried (MgSO4)
  10. customevaporated
  11. customto yield 452 g

Quellen und Nachweise

ORD-Eintrag
ord-e8beb3c22c5147819fa984e68643d425
Quelldatensatz
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04006179

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