Reaktion #54824
ord-84ca3aebe1814c88ba37e42ba26860be
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.ADDITIONTo this solution is added a solution of 56.7 g
- 2workup.ADDITIONDuring the addition
- 3Temperaturwith gradual warming to room temperature over 30 hours
- 4SonstigeThe solvent is removed in vacuo
- 5workup.DISTILLATIONThe residue is fractionally distilled
Vorschrift
Ethyl p-cyclohexylphenylglyoxylate, 49.5 g. (0.19 mole) and 6.1 g. of iodine are dissolved in 100 ml. of carbon tetrachloride. To this solution is added a solution of 56.7 g. (0.8 mole) of chlorine dissolved in 500 ml. of carbon tetrachloride over a period of 3 hours. During the addition, the temperature of the reaction mixture is maintained at 0° C. The mixture is stirred for 3 hours and allowed to stand with gradual warming to room temperature over 30 hours. The solvent is removed in vacuo. The residue is fractionally distilled to obtain ethyl 3,5-dichloro-4-cyclohexylphenylglyoxylate.