Ethyl formate → 2-(2,3-Dichlorophenyl)-3-oxo-propionitrile

HRID 234926

Reaktionsgleichung

Reaktionsgleichung von HRID 234926
C[CH2:2][O-:3].[Na+].[Cl:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:13][C:14]#[N:15].C(OCC)=O>C(O)C>[Cl:5][C:6]1[C:11]([Cl:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH:13]([CH:2]=[O:3])[C:14]#[N:15]

Komponenten

5

Edukt 3

HCID 8025Ethyl formate2×HCID 229020Benzeneacetonitrile, 2,3-dichloro-HCID 2723922Sodium ethoxide

Produkt 1

HCID 197051252-(2,3-Dichlorophenyl)-3-oxo-propionitrileAusbeute 45 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of NaOEt (from 3.63 gms Na) in ethanol (500 ml) was added 2,3-dichlorophenylacetonitrile (Example 14.3) in ethanol (150 ml). Ethyl formate (16.67 gms) was then added and the mixture stirred at 80° C. for 45 minutes, before adding a further quantity of ethyl formate (2.78 gms). After stirring at 80° C. for a further 1.5 hours, the precipitate was filtered off and dried in vacuo. The solid was dissolved in water, filtered, acidified with concentrated hydrochloric acid and the precipitate filtered off and dried in vacuo, 14.35 gms, 45% yield.

Aufarbeitung

  1. stirringAfter stirring at 80° C. for a further 1.5 hours
  2. filtrationthe precipitate was filtered off
  3. customdried in vacuo
  4. dissolutionThe solid was dissolved in water
  5. filtrationfiltered
  6. filtrationthe precipitate filtered off
  7. customdried in vacuo, 14.35 gms, 45% yield

Quellen und Nachweise

ORD-Eintrag
ord-52fac0f666914fbd8c525fb4448e1779
Quelldatensatz
uspto-grants-1997_01
Patentnummer
US05597827

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