반응 #63547

ord-ed624e9c145b44959ccc22e3d6dbe760

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04766145uspto-grants-1988_08