Sodium hydride → HCID 14612522, Verbindung

HRID 1031580Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1031580
[H-].[Na+].[CH2:3]([O:5][C:6](=[O:25])[C:7](=[CH:19][NH:20][C:21]([CH3:24])([CH3:23])[CH3:22])[C:8]([C:10]1[CH:15]=[C:14]([F:16])[C:13]([F:17])=[CH:12][C:11]=1F)=[O:9])[CH3:4]>O1CCOCC1>[CH2:3]([O:5][C:6]([C:7]1[C:8](=[O:9])[C:10]2[C:11](=[CH:12][C:13]([F:17])=[C:14]([F:16])[CH:15]=2)[N:20]([C:21]([CH3:24])([CH3:23])[CH3:22])[CH:19]=1)=[O:25])[CH3:4]

Komponenten

4

Edukt 2

HCID 24758Sodium hydrideHCID 178471998HCID 178471998, Verbindung

Produkt 1

HCID 14612522HCID 14612522, VerbindungAusbeute 94,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

There was added 1.1 g (27 mmoles) of 60% sodium hydride portionwise, at a temperature between 18° C. to 22° C., to a suspension of 7.22 g (21.9 mmoles) of 3-(2,4,5-trifluorophenyl)-3-oxo-2-(((1,1-dimethylethyl)amino)methylene)propanoic acid ethyl ester in 73 mL of anhydrous dioxane. An exothermic reaction occured. After stirring at room temperature during 1 hour, the resulting mixture was evaporated to dryness, and taken up with CH2Cl2 (150 mL) and H2O (200 mL). After decantation the organic layer was dried over MgSO4. Evaporation of dichloromethane gave 6.41 g of an amorphous solid which was washed twice with water to yield 6.08 g of titled compound.

Aufarbeitung

  1. customAn exothermic reaction
  2. customthe resulting mixture was evaporated to dryness
  3. dry with materialAfter decantation the organic layer was dried over MgSO4
  4. customEvaporation of dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-890515fef6614f90acff898cb2bbe266
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04954507

Notizen zur Reaktion

Wird geladen…