Réaction #725918
ord-78255972c4214702b3f50077c05af978
Équation de réaction
Réactifs
Aucun
Solvants
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Autrefor 1½ hours
- 2AutreDuring HCl gas bubbling the temp
- 3Autrerose to 60° C
- 4AutreThe crude reaction mass
- 5ExtractionCrude 48 was extracted into chloroform
- 6Séchagedried over Na2SO4
- 7workup.DISTILLATIONdistilled
- 8Autrepurified by column chromatography on silica gel
Mode opératoire
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.