반응 #1005940

반응 방정식

chloroacetone

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

potassium carbonate

sodium iodide

lithium chloride

→

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

용매

DMF

반응 조건

후처리

1. 1
   추출extracted with ethyl acetate three times
2. 2
   세척The combined extracts have been washed with 10% lithium chloride solution twice
3. 3
   건조dried with sodium sulfate
4. 4
   기타After removal of the solvent in vacuo the crude product
5. 5
   기타has been purified by chromatography on silica

실험 절차

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.

출처