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Acetic Anhydride → (4-Ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate

HRID 979861
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 979861
[C:1]([O:4][C:5](=[O:7])[CH3:6])(=O)[CH3:2].[CH2:8]([O:10][C:11]1[C:16](C)=[CH:15][N+:14]([O-])=[C:13](C)[C:12]=1[CH3:20])[CH3:9]>C(Cl)(Cl)Cl>[C:5]([O:4][CH2:1][C:2]1[C:16]([CH3:15])=[C:11]([O:10][CH2:8][CH3:9])[C:12]([CH3:20])=[CH:13][N:14]=1)(=[O:7])[CH3:6]
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Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 221514664-Ethoxy-2,3,5-trimethylpyridine 1-oxide

Produkt 1

HCID 22151469(4-Ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

75 ml of acetic anhydride were added dropwise at room temperature to a solution of 31.3 g of 4-ethoxy-2,3,5-trimethylpyridine 1-oxide in 100 ml of chloroform. After boiling under reflux for 16 hours the solution was evaporated, the residue was dissolved in 100 ml of toluene and again evaporated. The residue was taken up in 250 ml of ethyl acetate, whereupon it was extracted three times with 100 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 170 g of silica gel with ether. There was obtained (4-ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate in the form of an oil.

Aufarbeitung

  1. temperatureunder reflux for 16 hours the solution
  2. customwas evaporated
  3. dissolutionthe residue was dissolved in 100 ml of toluene
  4. customagain evaporated
  5. extractionwas extracted three times with 100 ml of saturated sodium bicarbonate solution
  6. dry with materialThe organic phase was dried over sodium sulfate
  7. customevaporated in vacuo
  8. customThe product was chromatographed on 170 g of silica gel with ether

Quellen und Nachweise

ORD-Eintrag
ord-1ffbaa5db98e4272b0babdf4cddbeaf1
Quelldatensatz
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04634710

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