Реакция #1005940

Уравнение реакции

chloroacetone

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

potassium carbonate

sodium iodide

lithium chloride

→

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

Растворители

DMF

Условия реакции

Обработка

1. 1
   Экстракцияextracted with ethyl acetate three times
2. 2
   ПромывкаThe combined extracts have been washed with 10% lithium chloride solution twice
3. 3
   Сушкаdried with sodium sulfate
4. 4
   ДругоеAfter removal of the solvent in vacuo the crude product
5. 5
   Другоеhas been purified by chromatography on silica

Методика

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.

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