Reaktion #2156155

Reaktionsgleichung

ethyl 2-ethoxy-4-fluorobenzoate

sulfuric acid

Potassium nitrate

→

title compound

Ethyl 2-ethoxy-4-fluoro-5-nitrobenzoate

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Temperaturunder cooling with ice
3. 3
   Temperaturunder cooling with ice
4. 4
   SonstigeThe reaction liquid
5. 5
   Filtrationthe precipitated crystals were recovered by filtration
6. 6
   Waschenwashed with water
7. 7
   SonstigeRecrystallizing the crystals from tert-butyl methyl ether-hexane mixed solvent

Vorschrift

In nitrogen atmosphere, to ethyl 2-ethoxy-4-fluorobenzoate as synthesized in above Production Example 31, 6.51 g, conc. sulfuric acid 34 mL was added under cooling with ice. Potassium nitrate 3.26 g was further added little by little, under cooling with salt-ice, followed by stirring for 3.4 hours under cooling with ice. The reaction liquid was poured in ice water, and the precipitated crystals were recovered by filtration and washed with water. Recrystallizing the crystals from tert-butyl methyl ether-hexane mixed solvent, 4.49 g of the title compound was obtained.

Quelle