反应详情

38.6 g (0.20 mole) of 2.5-dichloro-3-nitropyridine, 41.2 g (0.21 mole) of methyl 2-(4-hydroxyphenoxy)propionate, 400 ml of acetonitrile, 35.9 g (0.26 mole) of potassium carbonate and 0.33 g (0.002 mole) of potassium iodide are heated for 13 hours to 80° C. The reaction mixture is filtered and the filter cake is washed with acetonitrile. The filtrate is concentrated by evaporation and the residue is taken up in 500 ml of methlyene chloride. After treating the solution with 15 g of activated carbon, it is filtered through a layer of silica gel and the filtrate is concentrated by evaporation. The residue is crystallised from a mixture of hexane and ethyl acetate, affording 65.7 g (93.1% of theory) of methyl 2-[4-(5-chloro-3-nitropyridin-2-yloxy)phenoxy]propionate with a melting point of 91°-92° C.

1. filtrationThe reaction mixture is filtered
2. washthe filter cake is washed with acetonitrile
3. concentrationThe filtrate is concentrated by evaporation
4. additionAfter treating the solution with 15 g of activated carbon, it
5. filtrationis filtered through a layer of silica gel
6. concentrationthe filtrate is concentrated by evaporation
7. customThe residue is crystallised from a mixture of hexane and ethyl acetate