反応 #1005940

反応方程式

chloroacetone

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

potassium carbonate

sodium iodide

lithium chloride

→

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

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted with ethyl acetate three times
2. 2
   洗浄The combined extracts have been washed with 10% lithium chloride solution twice
3. 3
   乾燥dried with sodium sulfate
4. 4
   その他After removal of the solvent in vacuo the crude product
5. 5
   その他has been purified by chromatography on silica

実験手順

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.

出典