Sodium hydride → HCID 131711241, Verbindung

HRID 127782

Reaktionsgleichung

Reaktionsgleichung von HRID 127782
[H-].[Na+].[CH2:3]([CH:7]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:5][CH3:6].[Na].Cl([F:23])(=O)(=O)=O>C1(C)C=CC=CC=1>[CH2:11]([O:10][C:8](=[O:9])[CH:7]([CH2:3][CH:4]([F:23])[CH2:5][CH3:6])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH3:12]

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 67244Diethyl butylmalonateHCID 5360545Sodium

Produkt 1

HCID 131711241HCID 131711241, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a suspension of sodium hydride (1.08 mol) in 1200 ml of toluene was added dropwise 235 g (1.08 mol) of diethyl n-butylmalonate. To the resulting clear solution of the sodium salt was then bubbled perchloryl fluoride while the the temperature was maintained below 10° C. When the calculated amount of perchloryl fluoride had been added a stream of argon was bubbled through the solution for a short period of time. The mixture was filtered and the toluene removed under reduced pressure. The remaining oil was distilled to give 223 g, b.p. 78° (0.1 mmHg) of diethyl-2-fluoro-n-butylmalonate.

Aufarbeitung

  1. customwas bubbled through the solution for a short period of time
  2. filtrationThe mixture was filtered
  3. customthe toluene removed under reduced pressure
  4. distillationThe remaining oil was distilled

Quellen und Nachweise

ORD-Eintrag
ord-9a50b1d3a2c54a0cbea0fdc3245fad0f
Quelldatensatz
uspto-grants-1981_03
Patentnummer
US04256911

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