反应 #96164

ord-192fe84647684fc38c7548455c798d5e

反应方程式

C(=C1CCCCO1)[P+](c1ccccc1)(c1ccccc1)c1ccccc1.[Cl-]
[(tetrahydro-2H-pyran-2-ylidene)methyl]triphenylphosphonium chloride
O=CC1CCCCC1
cyclohexanecarbaldehyde
O=C(C=CC1CCCCC1)CCCCCl
1-cyclohexyl-7-chloro-1-hepten-3-one

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度This suspension was maintained under a nitrogen atmosphere
  2. 2
    温度was refluxed for about 4 hours until a clear solution
  3. 3
    其他formed
  4. 4
    其他xylene was removed at a temperature of about 60° C. and under reduced pressure
  5. 5
    其他leaving a product mixture
  6. 6
    其他This mixture was separated chromatographically on a silica column

实验过程

2 parts of [(tetrahydro-2H-pyran-2-ylidene)methyl]triphenylphosphonium chloride and 1.2 parts of cyclohexanecarbaldehyde were combined in 45 parts of xylene. This suspension was maintained under a nitrogen atmosphere and was refluxed for about 4 hours until a clear solution formed. After cooling the solution to room temperature, xylene was removed at a temperature of about 60° C. and under reduced pressure, leaving a product mixture. This mixture was separated chromatographically on a silica column using as the elution solvent 50 percent by volume of Skelly B in benzene, to yield 1-cyclohexyl-7-chloro-1-hepten-3-one.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04347192uspto-grants-1982_08