反应 #318647

反应方程式

N-allylaniline

1,1,3,3-tetramethyldisiloxane

carbon black

→

1,3-bis(N-phenyl-3-aminopropyl)-1,1,3,3-tetramethyldisiloxane

反应条件

后处理

1. 1
   其他equipped
2. 2
   温度with reflux condenser, nitrogen inlet
3. 3
   温度The contents of the reaction are heated
4. 4
   温度maintained
5. 5
   workup.STIRRINGwhile stirring, at approximately 70° C., for a period of ten hours
6. 6
   其他completion of the reaction
7. 7
   workup.STIRRINGstirred overnight at room temperature
8. 8
   过滤The product is filtered through silica gel
9. 9
   洗涤the filter cake washed with toluene
10. 10
    其他Volatile fractions are removed
11. 11
    其他by stripping under vacuum at 150° C.
12. 12
    其他to give a slightly colored oil
13. 13
    workup.DISTILLATIONThe oil is further purified by vacuum distillation at <1 torr at 223°-230° C

实验过程

N-allylaniline (0.200 mole) and 1,1,3,3-tetramethyldisiloxane (0.100 mole) are introduced along with 0.05 g hexachloroplatinic acid into a 100 ml cylindrical glass reactor equipped with reflux condenser, nitrogen inlet, and stir bar. The contents of the reaction are heated and maintained while stirring, at approximately 70° C., for a period of ten hours. The IR spectrum of the resulting viscous oil shows no peaks corresponding to Si-H, indicating completion of the reaction. The crude product is mixed with carbon black and stirred overnight at room temperature. The product is filtered through silica gel and the filter cake washed with toluene. Volatile fractions are removed by stripping under vacuum at 150° C. to give a slightly colored oil. The oil is further purified by vacuum distillation at <1 torr at 223°-230° C. The yield of 1,3-bis(N-phenyl-3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is virtually quantitative.

来源