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Sodium Hydroxide → HCID 12634259, Verbindung

HRID 1112718
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1112718
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[C:15]([NH:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])(=O)[C:16]([CH3:19])([CH3:18])[CH3:17].[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:17][C:16]([C:15]1[O:24][C:23]([O:25][CH2:26][CH3:27])=[CH:22][N:21]=1)([CH3:19])[CH3:18]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 3622015HCID 3622015, Verbindung

Produkt 1

HCID 12634259HCID 12634259, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

To a vigorously-stirred slurry of phosphorus pentoxide (163.8 g., 1.15 mole) in chloroform (600 ml.) maintained under a nitrogen atmosphere is added slowly a solution of ethyl N-pivaloylglycinate (107.8 g., 0.576 mole) in chloroform (350 ml.). Upon completing the addition, the reaction mixture is stirred and heated at reflux under a nitrogen atmosphere for 14 hours. The cooled reaction mixture is treated with 20% sodium hydroxide (800 ml.), vigorously stirred for 1/2 hour and allowed to separate into two phases. After discarding the aqueous phase, the organic phase is washed with water and saturated brine, dried over sodium sulfate and filtered. Distillation of the filtrate provides 2-(1,1-dimethylethyl)-5-ethoxyoxazole as a pale yellow liquid (64 g., 66%), b.p. 58°-64° C./0.7 mm.

Aufarbeitung

  1. additionthe addition
  2. temperatureheated
  3. temperatureat reflux under a nitrogen atmosphere for 14 hours
  4. customThe cooled reaction mixture
  5. stirringvigorously stirred for 1/2 hour
  6. customto separate into two phases
  7. washthe organic phase is washed with water and saturated brine
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. distillationDistillation of the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-6874b87b4c1e465aa354ef167fc98571
Quelldatensatz
uspto-grants-1978_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04123537

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