反应 #1435719

反应方程式

potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide

cyclopentadienyl zirconium trichloride

dimethoxyethane

→

cyclopentadienyl ((2-trimethylsiloxy-ethyl)-cyclopentadienyl) zirconium dichloride

收率 27.0%

溶剂

toluene

toluene

反应条件

后处理

1. 1
   workup.ADDITIONis added
2. 2
   workup.ADDITIONThe addition
3. 3
   其他is carried out at −78° C
4. 4
   其他An orange-brown suspension is immediately formed
5. 5
   温度it is maintained
6. 6
   workup.WAITthen it is left
7. 7
   过滤it is filtered
8. 8
   浓缩The obtained orange solution is concentrated up to 5 ml and hexane
9. 9
   workup.ADDITIONis added, so that a brown solid
10. 10
    其他is obtained

实验过程

To a suspension of 3.52 g (10 mmol) of an adduct of cyclopentadienyl zirconium trichloride with dimethoxyethane in toluene, a suspension of 2.2 g (10 mmol) of potassium (2-trimethylsiloxy-ethyl)-cyclopentadienide in toluene is added. The addition is carried out at −78° C. An orange-brown suspension is immediately formed; it is maintained under stirring for 12 hours; then it is left settling and it is filtered. The obtained orange solution is concentrated up to 5 ml and hexane is added, so that a brown solid is obtained. (1.1 g, 2.7 mmol. Yield: 27%). 1H-NMR: 6.00 (t, 2H), 5.87 (s, 5H), 5.67 (t, 2H), 3.66 (t, 2H), 2.92 (t, 2H), 0.11 (s, 9H). Mass spectrum. M+-65: (343): 33%.

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