Réaction #1005940

Équation de réaction

chloroacetone

1-(4-chlorophenyl)pyrazol-3-ol

potassium carbonate

sodium iodide

lithium chloride

→

1-[1-(4-Chlorophenyl)pyrazol-3-yl]oxypropan-2-one

Solvants

DMF

Conditions de réaction

Traitement

1. 1
   Extractionextracted with ethyl acetate three times
2. 2
   LavageThe combined extracts have been washed with 10% lithium chloride solution twice
3. 3
   Séchagedried with sodium sulfate
4. 4
   AutreAfter removal of the solvent in vacuo the crude product
5. 5
   Autrehas been purified by chromatography on silica

Mode opératoire

5.50 g (28.3 mmol) 1-(4-chlorophenyl)pyrazol-3-ol, 3.91 g (28.3 mmol) potassium carbonate and 50 mg sodium iodide in 30 ml DMF have been stirred for 5 min at ambient temperature. Then 2.62 g (28.3 mmol) chloroacetone have been added dropwise while stirring which was continued at 60° C. for 5 h. The mixture was poured into excess 10% aqueous lithium chloride solution and extracted with ethyl acetate three times. The combined extracts have been washed with 10% lithium chloride solution twice and dried with sodium sulfate. After removal of the solvent in vacuo the crude product has been purified by chromatography on silica. Yield 6.5 g. The product was used for the next step.

Source