反应 #2320146

ord-7d7ee3507aef4eb1b1de0440e10cbfe9

反应方程式

Clc1cccc(I)c1Cl
1,2-Dichloro-3-iodobenzene
C#C[Si](C)(C)C
trimethylsilylacetylene
C[Si](C)(C)C#Cc1cccc(Cl)c1Cl
[(2,3-dichlorophenyl)ethynyl](trimethyl)silane

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度at reflux for 45 minutes
  3. 3
    其他was then partitioned between diethyl ether and saturated sodium chloride
  4. 4
    干燥The organic phase was dried with sodium sulfate
  5. 5
    过滤filtered through celite
  6. 6
    浓缩the filtrate was concentrated under reduced pressure

实验过程

1,2-Dichloro-3-iodobenzene (4.95 g, 18.1 mmol), trimethylsilylacetylene (2 g, 20 mmol), bis(triphenylphosphine)palladium(II)chloride (245 mg, 0.35 mmol), and copper(I)iodide (45 mg, 0.24 mmol) were combined in triethylamine (120 mL) and heated at reflux for 45 minutes. The mixture was allowed to cool to room temperature and was then partitioned between diethyl ether and saturated sodium chloride. The organic phase was dried with sodium sulfate, filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was taken directly on to the next step.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07709469B2uspto-grants-2010_05