반응 #217752

반응 방정식

ethyl salicylate

tetrabutylammonium hydroxide

→

Tetrabutylammonium Salicylate

용매

water

반응 조건

후처리

1. 1
   온도A glass flask with reflux condenser, heatable oil bath, mechanical stirrer
2. 2
   workup.STIRRINGIt was stirred at 60° C. for one hour (the contents of the flask
3. 3
   온도Then the reaction mixture was cooled
4. 4
   workup.DISTILLATIONthe water was distilled off under reduced pressure, 20 mbar, at 30-45° C
5. 5
   기타was taken up at 60° C. in 200 ml of toluene
6. 6
   workup.DISTILLATIONSubsequently the mixture was redistilled
7. 7
   기타The residue was recrystallized from 50 ml of butyl acetate
8. 8
   여과The product was filtered off
9. 9
   세척washed with butyl acetate
10. 10
    기타dried at 80° C.
11. 11
    기타10 mbar in a vacuum drying cabinet
12. 12
    기타This gave a white solid

실험 절차

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 become 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 having a melting point of 93° C.

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