تفاعل #63547

ord-ed624e9c145b44959ccc22e3d6dbe760

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04766145uspto-grants-1988_08