Reacción #162831

Ecuación de reacción

1-cyclopropyl-3-(2-fluoro-4-iodophenyl)urea

malonic acid

acetic anhydride

acetyl chloride

→

1-cyclopropyl-3-(2-fluoro-4-iodophenyl)pyrimidine-2,4,6-trione

Rendimiento 82.3%

Disolventes

water toluene

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturato cool to room temperature
2. 2
   workup.STIRRINGwith stirring
3. 3
   FiltraciónThe precipitated crystals were collected by filtration
4. 4
   Otrodried

Procedimiento

To 1-cyclopropyl-3-(2-fluoro-4-iodophenyl)urea 48 (61.0 g) obtained in Step 1 and malonic acid 4 (19.9 g) were added acetic anhydride (300 ml) and acetyl chloride (27.2 ml), and the mixture was stirred under a nitrogen atmosphere at 60° C. for 3 hrs. After allowing to cool to room temperature, the reaction mixture was added dropwise to water-toluene [2:1 (volume ratio), 900 ml] with stirring. The precipitated crystals were collected by filtration and dried to give 1-cyclopropyl-3-(2-fluoro-4-iodophenyl)pyrimidine-2,4,6-trione 49 (60.9 g, yield 82%) as pale-yellow crystals.

Fuente