反应详情

A solution of 1,5-dichloro-2,4-dinitrobenzene (2.0 g), ethyl glycolate (1.32 g) and anhydrous potassium carbonate (0.88 g) and TDA-1 (0.27 g) in acetonitrile (10 g) was refluxed for 5 hours. After cooling, the reaction mixture was diluted with 3% hydrochloric acid (200 ml) and extracted with ethyl acetate. The organic layer was washed with 5% sodium carbonate solution, water and saturate sodium chloride solution in order, dried over magnesium sulfate, filtered and concentrated. The precipitated crystals were collected by filtration and recrystallized from methanol to give ethyl 2,4-dinitro-5-chlorophenoxyacetate (1.9 g; yield, 73.9%). M.P., 129°-130° C.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with 5% sodium carbonate solution, water
4. concentrationsaturate sodium chloride solution in order
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. filtrationThe precipitated crystals were collected by filtration
9. customrecrystallized from methanol