反应 #2460319

ord-06046a032b19462a939e55a60924d148

反应方程式

ClCc1ccc(CCl)cc1
α,α′-dichloro-p-xylene
CCOP(OCC)OCC
triethyl phosphite
CCOP(=O)(Cc1ccc(CP(=O)(OCC)OCC)cc1)OCC
tetraethyl p-xylylenebisphosphonate

反应条件

温度
180°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他white crystals were formed immediately
  2. 2
    温度Then the mixture was cooled at 0° C.
  3. 3
    其他the product was collected
  4. 4
    洗涤washed three times with 40 ml of hexanes
  5. 5
    其他isolated in 94.4% (40.8 g)
  6. 6
    其他yield

实验过程

A mixture of α,α′-dichloro-p-xylene (20 g, 0.114 mol) and triethyl phosphite (60 ml) was refluxed at 180° C. overnight. 80 ml of hexanes was added, and white crystals were formed immediately. Then the mixture was cooled at 0° C., and the product was collected, washed three times with 40 ml of hexanes and isolated in 94.4% (40.8 g) yield.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07459106B2uspto-grants-2008_12