Acetic Anhydride → 2-(2,4-Dichloro-5-fluorobenzoyl)3-methoxy-acrylonitrile

HRID 2118796

Reaktionsgleichung

Reaktionsgleichung von HRID 2118796
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[C:10]([F:14])=[CH:9][C:3]=1[C:4]([CH2:6][C:7]#[N:8])=[O:5].[C:15]([O:18][C:19](=O)C)(=O)C>>[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[C:10]([F:14])=[CH:9][C:3]=1[C:4]([C:6](=[CH:15][O:18][CH3:19])[C:7]#[N:8])=[O:5]

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 136307213-(2,4-Dichloro-5-fluorophenyl)-3-oxopropanenitrile

Produkt 1

HCID 537325472-(2,4-Dichloro-5-fluorobenzoyl)3-methoxy-acrylonitrileAusbeute 99 %

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of 21 g of 2,4-dichloro-5-fluorobenzoyl-acetonitrile, 19.2 g of methyl o-formate and 23.1 g of acetic anhydride is refluxed at a bath temperature of 150° C. for 3 hours. The volatile constituents are then distilled off under a waterpump vacuum and finally under a fine vacuum at a bath temperature of 120° C. 24.5 g (99%) of 2-(2,4-dichloro-5-fluorobenzoyl)-3-methoxy-acrylonitrile are obtained. A sample recrystallized from toluene gives colorless crystals of melting point 159° C.

Aufarbeitung

  1. distillationThe volatile constituents are then distilled off under a waterpump vacuum and finally under a fine vacuum at a bath temperature of 120° C

Quellen und Nachweise

ORD-Eintrag
ord-fa83ee9951514373a2c23b785b3dfbfc
Quelldatensatz
uspto-grants-1987_07
Patentnummer
US04680401

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