反応 #2045003

反応方程式

Paracetamol

K2CO3

ethyl bromoacetate

→

13

収率 80.1%

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

収率 80.1%

溶媒

acetone

反応条件

後処理

1. 1
   温度refluxed for 16 hours
2. 2
   workup.DISTILLATIONAcetone was distilled off
3. 3
   workup.ADDITIONwater (5 liter) was added
4. 4
   ろ過Crude 13 was filtered
5. 5
   その他dried
6. 6
   その他recrystallised from a mixture of toluene:hexane (1:5)

実験手順

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.

出典