反应详情

温度

60 °C

A glass flask with reflux condenser, heatable oil bath, mechanical stirrer and internal thermometer was charged at room temperature with 35.90 g of ethyl salicylate and 282.13 g of water and these components were stirred together thoroughly. Subsequently 139.98 g of tetrabutylammonium hydroxide (40% strength in water) were added and the reaction mixture was heated to 60° C. It was stirred at 60° C. for one hour (the contents of the flask became clear). Then the reaction mixture was cooled and the water was distilled off under reduced pressure, 20 mbar, at 30-45° C. The residue was taken up at 60° C. in 200 ml of toluene. Subsequently the mixture was redistilled. The residue was recrystallized from 50 ml of butyl acetate. The product was filtered off, washed with butyl acetate and dried at 80° C. and 10 mbar in a vacuum drying cabinet. This gave a white solid.

1. temperatureA glass flask with reflux condenser, heatable oil bath, mechanical stirrer
2. stirringIt was stirred at 60° C. for one hour (the contents of the flask
3. temperatureThen the reaction mixture was cooled
4. distillationthe water was distilled off under reduced pressure, 20 mbar, at 30-45° C
5. customwas taken up at 60° C. in 200 ml of toluene
6. distillationSubsequently the mixture was redistilled
7. customThe residue was recrystallized from 50 ml of butyl acetate
8. filtrationThe product was filtered off
9. washwashed with butyl acetate
10. customdried at 80° C.
11. custom10 mbar in a vacuum drying cabinet
12. customThis gave a white solid