Dimethylformamide → HCID 19096639, Verbindung

HRID 486842Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 486842
[N-:1]=[N+:2]=[N-:3].[Na+].CN(C=O)C.[CH3:10][C:11]1([CH3:23])[O:16][C:15](=[O:17])[CH:14]=[C:13]([CH2:18][C:19](=[O:22])[CH2:20]Cl)[O:12]1>C(OCC)(=O)C>[CH3:10][C:11]1([CH3:23])[O:16][C:15](=[O:17])[CH:14]=[C:13]([CH2:18][C:19](=[O:22])[CH2:20][N:1]=[N+:2]=[N-:3])[O:12]1

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 33557Sodium AzideHCID 149448286-(3-Chloro-2-oxopropyl)-2,2-dimethyl-2H,4H-1,3-dioxin-4-one

Produkt 1

HCID 19096639HCID 19096639, VerbindungAusbeute 82,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

195 mg (3.0 mmol) of sodium azide were added to 2 ml of a DMF solution containing 328 mg (1.5 mmol) of 2,2-dimethyl-6-(3-chloro-2-oxopropyl)-1,3-dioxin-4-one prepared in Example 1, followed by stirring at room temperature for 10 minutes. Afterward, the solution was poured into ice water, extracted with ether, and then dried with anhydrous magnesium sulfate. After ether was distilled off, the residue was then subjected to column chromatography (an eluent of hexane:ethyl acetate=1:1), thereby obtaining 278 mg (yield 82%) of 2,2-dimethyl-6-(3-azido-2-oxopropyl)-1,3-dioxin-4-one.

Aufarbeitung

  1. extractionextracted with ether
  2. dry with materialdried with anhydrous magnesium sulfate
  3. distillationAfter ether was distilled off

Quellen und Nachweise

ORD-Eintrag
ord-4288d4b185404b74b38d3e5847ca867d
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05292891

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