Reaktion #2045035

Reaktionsgleichung

2-(4-Nitro-phenoxy)-propionic acid

ethylene glycol

HCl

→

48

Ausbeute 56.8%

2-(4-Nitro-phenoxy)-propionic acid 2-hydroxy-ethyl ester

Ausbeute 56.8%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigefor 1½ hours
2. 2
   SonstigeDuring HCl gas bubbling the temp
3. 3
   Sonstigerose to 60° C
4. 4
   SonstigeThe crude reaction mass
5. 5
   ExtraktionCrude 48 was extracted into chloroform
6. 6
   Trocknendried over Na2SO4
7. 7
   workup.DISTILLATIONdistilled
8. 8
   Sonstigepurified by column chromatography on silica gel

Vorschrift

To a mixture of 2-(4-Nitro-phenoxy)-propionic acid 47 (45 g, 213 mol) and ethylene glycol (135 ml) was passed dry HCl gas for 1½ hours. During HCl gas bubbling the temp. rose to 60° C. The crude reaction mass was poured onto cold water (600 ml). Crude 48 was extracted into chloroform, dried over Na2SO4, distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 48 (28 g, 56.8%) as a syrup.

Quelle