反应详情

温度

5 °C

5.9 g (0.043 mol) of sodium dihydrogen phosphate monohydrate in 70 ml of water, 20.5 g (0.181 mol) of 30% strength hydrogen peroxide solution and 27.3 g (0.241 mol) of 80% strength sodium chlorite solution were added in succession to a solution of 40.0 g (0.172 mol) of methyl 2,4-dichloro-3-formylbenzoate and 500 ml of acetonitrile. The reaction solution was stirred for 1 hour at 5° C. and for 12 hours at room temperature. It was subsequently brought to pH 1 with 10% strength hydrochloric acid, and 500 ml of 40% strength sodium hydrogen sulfite solution were added. After the mixture had been stirred for 1 hour at room temperature, the aqueous phase was extracted three times with ethyl acetate, and the combined organic phases were washed with 1.0 l of 10% strength sodium hydrogen sulfite solution and subsequently dried. After the solvent had been distilled off, 40.0 g of methyl 2,4-dichloro-3-hydroxycarbonylbenzoate were obtained.

1. additionwere added
2. stirringAfter the mixture had been stirred for 1 hour at room temperature
3. extractionthe aqueous phase was extracted three times with ethyl acetate
4. washthe combined organic phases were washed with 1.0 l of 10% strength sodium hydrogen sulfite solution
5. customsubsequently dried
6. distillationAfter the solvent had been distilled off