反応 #63547

反応方程式

Oxalyl chloride

1-ethoxycarbonylcyclopropane carboxylic acid

1-Ethoxycarbonylcyclopropanecarboxylic acid

→

desired product

1-Ethoxycarbonylcyclopropanecarbonyl chloride

溶媒

benzene

反応条件

後処理

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

実験手順

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.

出典