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Acetic Anhydride → HCID 20465612, Verbindung

HRID 328834
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 328834
[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 70) 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 helix-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 produce 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 helix-packed fractionation column
  4. temperatureto maintain a constant volume until complete conversion of starting materials
  5. customto produce
  6. temperatureThe mixture is cooled
  7. custompartitioned between 2 l
  8. temperatureof cold water containing solid sodium bicarbonate to maintain a neutral pH
  9. washThe organic phase is washed with saturated brine
  10. dry with materialdried (MgSO4)
  11. customevaporated
  12. customto yield 452 g

Quellen und Nachweise

ORD-Eintrag
ord-23073027bc9f4efbbe648e977cfa3e32
Quelldatensatz
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04018811

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