반응 #170967

반응 방정식

methyl 2-chloropropionate

4-nitrophenol

K2CO3

sodium iodide

→

14

수율 31.0%

2-(4-Nitrophenoxy)-propionic acid methyl ester

수율 31.0%

용매

acetone

반응 조건

후처리

1. 1
   온도refluxed for 20 hours
2. 2
   workup.DISTILLATIONAcetone was distilled off
3. 3
   workup.ADDITIONwater (3 L) was added
4. 4
   여과Crude 14 was filtered
5. 5
   기타dried
6. 6
   기타recrystallised from a mixture of ethyl acetate:hexane (1:5)

실험 절차

To a mixture of 4-nitrophenol (200 grm, 1.439 mol), anhydrous K2CO3 (800 grm, 5.789 mol) and sodium iodide (10 g, 66.7 mmol) in anhydrous acetone (2.75 L) was added methyl 2-chloropropionate (264 g, 2.154 mol) and refluxed for 20 hours. Acetone was distilled off and water (3 L) was added. Crude 14 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 14 (100 g, 31%) as a white fluffy powder with a m.p between 83-84° C.

출처