反应详情

温度

10 °C

To a solution of crude 3-[3-(4-fluorophenyl)-1H-pyrazol-5-yl]propyl methanesulfonate (52 g, 0.122 mol), in 300 mL N,N′-Dimethylformamide is added at 10° C. sodium iodide (1.84 g, 12.2 mmol). Then, sodium hydride (60%, 5.4 g, 0.134 mol) is added portionwise and the mixture is stirred for 30 min at 10° C. followed by 1 h at room temperature. To the resulting brown suspension is added saturated ammonium chloride and the mixture is extracted with ethyl acetate. The extracts are dried and evaporated in vacuo. The obtained crude product is purified by trituration with 50 mL water+50 mL n-hexane. After drying of the solid in vacuo 22.9 g (90%) of the product is obtained and is being used without further purification in the next step.

1. waitfollowed by 1 h at room temperature
2. extractionthe mixture is extracted with ethyl acetate
3. customThe extracts are dried
4. customevaporated in vacuo
5. customThe obtained crude product
6. customis purified by trituration with 50 mL water+50 mL n-hexane
7. dry with materialAfter drying of the solid in vacuo 22.9 g (90%) of the product
8. customis obtained
9. customis being used without further purification in the next step