반응 #589016

반응 방정식

methyl 2-chloropropionate

paracetamol

K2CO3

sodium iodide

→

8

2-(4-Acetylamino-phenoxy)-propionic acid methyl ester

용매

acetone

반응 조건

후처리

1. 1
   온도refluxed for 80 hours
2. 2
   workup.DISTILLATIONThe acetone was distilled off
3. 3
   workup.ADDITIONwater (3 L) was added
4. 4
   추출Crude 8 was extracted into chloroform
5. 5
   건조dried over Na2SO4
6. 6
   workup.DISTILLATIONdistilled
7. 7
   workup.ADDITIONhexane (750 ml) was added
8. 8
   여과The solids were then filtered
9. 9
   기타recrystallised in methanol

실험 절차

To a mixture of paracetamol (150 g, 992 mmol), anhydrous K2CO3 (540 kg, 3.91 mol) and sodium iodide (18 gm, 120 mmol) in anhydrous acetone (3 L) was added methyl 2-chloropropionate (180 g, 1.469 mmol) and refluxed for 80 hours. The acetone was distilled off and water (3 L) was added. Crude 8 was extracted into chloroform, dried over Na2SO4, distilled and hexane (750 ml) was added. The solids were then filtered and recrystallised in methanol to give pure 8 (95 g, 40.4%) as a white powder with an m.p between 96.5-98.2° C.

출처