反应详情

温度

65 °C

To 2.6 g of chromium trichloride suspended in 50 ml of THF are successively added 30 ml of a 0.5M solution in THF of 2-chlorophenyliodozinc, 2.54 g of 2-nitro-5-fluorobenzaldehyde and 5.7 ml of trimethylsilyl chloride. The mixture is heated at 65° C. for 1 hour and then left at room temperature for 18 hours. 1M hydrochloric acid solution is added to the reaction medium, the precipitate formed is filtered off and the filtrate is concentrated. The residue is taken up in ethyl acetate and washed with water. The organic phase is dried over anhydrous sodium sulfate and concentrated. The residue is chromatographed on a column of silica gel, eluting with cyclohexane, to give 1 g of the expected product.

1. customthe precipitate formed
2. filtrationis filtered off
3. concentrationthe filtrate is concentrated
4. washwashed with water
5. dry with materialThe organic phase is dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue is chromatographed on a column of silica gel
8. washeluting with cyclohexane