Acetic Anhydride → HCID 18458647, Verbindung

HRID 2304808Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2304808
[OH:1][CH:2]1[C:7]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])=[CH:6][CH2:5][N:4]([CH3:20])[CH2:3]1.[C:21](OC(=O)C)(=[O:23])[CH3:22]>>[C:21]([O:1][CH:2]1[C:7]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])=[CH:6][CH2:5][N:4]([CH3:20])[CH2:3]1)(=[O:23])[CH3:22]

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 99256571,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

Produkt 1

HCID 18458647HCID 18458647, Verbindung

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

2.79 g (10 mmol) of 3(R,S)-hydroxy-1-methyl-4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine (VII) were dissolved in 15 ml of acetic anhydride and stirred at 100° C. for 4 h. The solution was then evaporated in vacuo in a rotary evaporator and the residue was dissolved in 10 ml of water, adjusted to pH>12 with sodium hydroxide solution and extracted twice with 20 ml of ethyl acetate each time. The combined organic phases were washed with 10 ml of saturated sodium chloride solution, then dried over sodium sulfate and evaporated in vacuo on a rotary evaporator.

Aufarbeitung

  1. customThe solution was then evaporated in vacuo in a rotary evaporator
  2. dissolutionthe residue was dissolved in 10 ml of water
  3. extractionextracted twice with 20 ml of ethyl acetate each time
  4. washThe combined organic phases were washed with 10 ml of saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo on a rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-b585caff145748e29dc194389e82d348
Quelldatensatz
uspto-grants-2002_08
Patentnummer
US06437136B1

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