反应详情

To a slurry of NaH (1.64 g, 60% suspension in mineral oil, 41.1 mmol) in DMSO (19 mL) stirred at room temperature, was added a solution of 1,3-dibromopropane (2.1 mL, 20.6 mmol) and (4-Bromo-2-fluoro-phenyl)-acetonitrile (4.0 g, 18.7 mmol) in diethyl ether (10 mL) slowly keeping the temprature of the reaction between 25 degrees Celsius and 35 degrees Celsius. Stir for two hours after the addition is complete, and pour into saturated ammonium chloride (150 mL). Add 100 ml of CH2Cl2 and separate the layers. Extract the aqueous phase with 2×50 mL CH2Cl2 and combine the organics. After drying the organic liquid over MgSO4, the solids were removed by filtration, and the liquid was concentrated to an oil. The oil was purified by flash chromatography to yield the desired product. Yield: 1.43 g, 30%.

1. customthe temprature of the reaction between 25 degrees Celsius and 35 degrees Celsius
2. additionafter the addition
3. customseparate the layers
4. extractionExtract the aqueous phase with 2×50 mL CH2Cl2
5. dry with materialAfter drying the organic liquid over MgSO4
6. customthe solids were removed by filtration
7. concentrationthe liquid was concentrated to an oil
8. customThe oil was purified by flash chromatography