Reaktion #63547

Reaktionsgleichung

Oxalyl chloride

1-ethoxycarbonylcyclopropane carboxylic acid

1-Ethoxycarbonylcyclopropanecarboxylic acid

→

desired product

1-Ethoxycarbonylcyclopropanecarbonyl chloride

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITthe stirring was continued at room temperature for another hour
2. 2
   EinengenThe reaction mixture was concentrated
3. 3
   workup.DISTILLATIONThe residue was purified by distillation
4. 4
   SonstigeA fraction collected at 91°-2° C./15 mm
5. 5
   workup.DISTILLATIONwas redistilled

Vorschrift

Oxalyl chloride (6.0 g. 47 mmol) was added to a stirred mixture of 1-ethoxycarbonylcyclopropane carboxylic acid (1a) (6 g, 38 mmol) in benzene (25 ml) plus two drops of dimethylformamide. After the gas evolution ceased, the stirring was continued at room temperature for another hour. The reaction mixture was concentrated. The residue was purified by distillation. A fraction collected at 91°-2° C./15 mm was redistilled to give the desired product.

Quelle