Hydrochloric Acid → Benzoylacetonitrile

Temperatur

60 °C

To a solution of acetonitrile (76 g) in DMSO (100 mL) was added methyl p-anisate (100 g) and the mixture was stirred with heating at 60° C. for one hour. The reaction mixture was allowed to cool, and cold water (500 mL) was added dropwise. The mixture was acidified with hydrochloric acid and the precipitated crystals were collected by filtration. The obtained crystals were extracted with ethyl acetate and the solvent was evaporated under reduced pressure. The residue was recrystallized from ethyl acetate to give benzoylacetonitrile (60 g) as colorless crystals. A solution of 2-chlorobenzaldehyde (1.7 g), 3-aminopyrazole (1.0 g) and benzoylacetonitrile (1.8 g) in acetonitrile (20 mL) was heated under reflux overnight. The reaction mixture was cooled to room temperature, and the precipitated crystals were collected by filtration to give the title compound (2.63 g) as colorless crystals.

1. temperatureto cool
2. filtrationthe precipitated crystals were collected by filtration
3. extractionThe obtained crystals were extracted with ethyl acetate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was recrystallized from ethyl acetate

ORD-Eintrag

ord-6a11c53e02c0491fb90c2cb30ff330c7

Quelldatensatz

uspto-grants-2005_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06977262B2