反应详情

To a solution of 19.1 g of ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoate in 100 ml of methanol is added dropwise a solution of 7.56 g of sodium hydroxide in 100 ml of water under ice-cooling. After stirring under ice-cooling for 20 minutes, the methanol is distilled off under reduced pressure. The solution is washed with ethyl acetate, made acid with 6 N hydrochloric acid and then extracted with ethyl acetate. After drying over anhydrous magnesium sulfate, the ethyl acetate is distilled off under reduced pressure. To the residue is added isopropyl ether. The obtained crystals are filtered with suction and dried to give 12.2 g of 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)-morpholino]-2,3,5-trifluorobenzoic acid in 68% yield, melting at 170°-172° C.

1. temperaturecooling
2. temperaturecooling for 20 minutes
3. distillationthe methanol is distilled off under reduced pressure
4. washThe solution is washed with ethyl acetate
5. extractionextracted with ethyl acetate
6. dry with materialAfter drying over anhydrous magnesium sulfate
7. distillationthe ethyl acetate is distilled off under reduced pressure
8. additionTo the residue is added isopropyl ether
9. filtrationThe obtained crystals are filtered with suction
10. customdried