反応 #217752

反応方程式

ethyl salicylate

tetrabutylammonium hydroxide

→

Tetrabutylammonium Salicylate

溶媒

water

反応条件

後処理

1. 1
   温度A 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
   温度Then the reaction mixture was cooled
4. 4
   workup.DISTILLATIONthe water was distilled off under reduced pressure, 20 mbar, at 30-45° C
5. 5
   その他was taken up at 60° C. in 200 ml of toluene
6. 6
   workup.DISTILLATIONSubsequently the mixture was redistilled
7. 7
   その他The residue was recrystallized from 50 ml of butyl acetate
8. 8
   ろ過The product was filtered off
9. 9
   洗浄washed with butyl acetate
10. 10
    その他dried at 80° C.
11. 11
    その他10 mbar in a vacuum drying cabinet
12. 12
    その他This gave a white solid

実験手順

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.

出典