Water → 3-(3-Nitro-phenyl)-acrylonitrile

HRID 1837515

Reaktionsgleichung

Reaktionsgleichung von HRID 1837515
[C:1]([CH2:3]P(=O)(OCC)OCC)#[N:2].[H-].[Na+].[N+:14]([C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][CH:24]=1)[CH:20]=O)([O-:16])=[O:15].O>O1CCCC1>[N+:14]([C:17]1[CH:18]=[C:19]([CH:20]=[CH:3][C:1]#[N:2])[CH:22]=[CH:23][CH:24]=1)([O-:16])=[O:15]

Komponenten

6

Edukt 4

HCID 962WaterHCID 74493-NitrobenzaldehydeHCID 24758Sodium hydrideHCID 75676Diethyl (cyanomethyl)phosphonate

Produkt 1

HCID 556693-(3-Nitro-phenyl)-acrylonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

At 0° C., 75.5 g of diethyl cyanomethylphosphonate dissolved in tetrahydrofuran are poured into a suspension of sodium hydride in tetrahydrofuran. After 30 minutes' contact at ambient temperature, 56 g of 3-nitrobenzaldehyde dissolved in tetrahydrofuran are poured in. After 1 hour, hydrolysis is carried out with 300 ml of water and then the solvent is concentrated. Following extraction with dichloromethane, washing the organic phase with water, drying over magnesium sulphate and concentration, the precipitate is taken up in diethyl ether and filtered off.

Aufarbeitung

  1. additionare poured in
  2. waitAfter 1 hour
  3. customhydrolysis
  4. concentrationthe solvent is concentrated
  5. extractionextraction with dichloromethane
  6. washwashing the organic phase with water
  7. dry with materialdrying over magnesium sulphate and concentration
  8. filtrationfiltered off

Quellen und Nachweise

ORD-Eintrag
ord-83ff63ba8c864af485b35e9f901d6e97
Quelldatensatz
uspto-grants-2004_08
Patentnummer
US06784183B2

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