Reaktion #170960

Reaktionsgleichung

4-nitrophenol

K2CO3

methyl chloroacetate

→

7

Ausbeute 72.5%

Methyl (4-Nitro phenoxy)acetate

Ausbeute 72.5%

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed for 12 hours
2. 2
   workup.DISTILLATIONAcetone was distilled off
3. 3
   workup.ADDITIONwater (1500 ml) was added
4. 4
   FiltrationCrude 7 was filtered
5. 5
   Sonstigedried
6. 6
   Sonstigerecrystallised from a mixture of ethyl acetate:hexane (1:5)

Vorschrift

To a mixture of 4-nitrophenol (100 g, 719 mmol) and anhydrous K2CO3 (400 gm, 2.894 mol) in anhydrous acetone (950 ml) was added methyl chloroacetate (114 g, 1.050 moles) and refluxed for 12 hours. Acetone was distilled off and water (1500 ml) was added. Crude 7 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 7 (110 g, 72.5%) as a white fluffy powder with an m.p between 97-98.4° C.

Quelle