반응 #54824

ord-84ca3aebe1814c88ba37e42ba26860be

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONTo this solution is added a solution of 56.7 g
  2. 2
    workup.ADDITIONDuring the addition
  3. 3
    온도with gradual warming to room temperature over 30 hours
  4. 4
    기타The solvent is removed in vacuo
  5. 5
    workup.DISTILLATIONThe residue is fractionally distilled

실험 절차

Ethyl p-cyclohexylphenylglyoxylate, 49.5 g. (0.19 mole) and 6.1 g. of iodine are dissolved in 100 ml. of carbon tetrachloride. To this solution is added a solution of 56.7 g. (0.8 mole) of chlorine dissolved in 500 ml. of carbon tetrachloride over a period of 3 hours. During the addition, the temperature of the reaction mixture is maintained at 0° C. The mixture is stirred for 3 hours and allowed to stand with gradual warming to room temperature over 30 hours. The solvent is removed in vacuo. The residue is fractionally distilled to obtain ethyl 3,5-dichloro-4-cyclohexylphenylglyoxylate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04150148uspto-grants-1979_04