반응 #725887

반응 방정식

Paracetamol

K2CO3

ethyl bromoacetate

→

13

수율 80.1%

(4-Acetylamino-phenoxy)-acetic acid ethyl ester

수율 80.1%

용매

acetone

반응 조건

후처리

1. 1
   온도refluxed for 16 hours
2. 2
   workup.DISTILLATIONAcetone was distilled off
3. 3
   workup.ADDITIONwater (5 liter) was added
4. 4
   여과Crude 13 was filtered
5. 5
   기타dried
6. 6
   기타recrystallised from a mixture of toluene:hexane (1:5)

실험 절차

To a mixture of Paracetamol (300 g, 1.984 mol), and anhydrous K2CO3 (1.80 Kg, 7.814 mmol) in anhydrous acetone (3 liters) was added ethyl bromoacetate (452 gr, 2.7 mol) and refluxed for 16 hours. Acetone was distilled off and water (5 liter) was added. Crude 13 was filtered, dried and recrystallised from a mixture of toluene:hexane (1:5) to give pure 13 (377 g, 80%) as a white shining powder. The melting point was found to be 104.2-106.2° C.

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