반응 #63547
ord-ed624e9c145b44959ccc22e3d6dbe760
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반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1workup.WAITthe stirring was continued at room temperature for another hour
- 2농축The reaction mixture was concentrated
- 3workup.DISTILLATIONThe residue was purified by distillation
- 4기타A fraction collected at 91°-2° C./15 mm
- 5workup.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.