반응 #318647

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N-allylaniline

1,1,3,3-tetramethyldisiloxane

carbon black

→

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

반응 조건

후처리

1. 1
   기타equipped
2. 2
   온도with reflux condenser, nitrogen inlet
3. 3
   온도The contents of the reaction are heated
4. 4
   온도maintained
5. 5
   workup.STIRRINGwhile stirring, at approximately 70° C., for a period of ten hours
6. 6
   기타completion of the reaction
7. 7
   workup.STIRRINGstirred overnight at room temperature
8. 8
   여과The product is filtered through silica gel
9. 9
   세척the filter cake washed with toluene
10. 10
    기타Volatile fractions are removed
11. 11
    기타by stripping under vacuum at 150° C.
12. 12
    기타to give a slightly colored oil
13. 13
    workup.DISTILLATIONThe oil is further purified by vacuum distillation at <1 torr at 223°-230° C

실험 절차

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.

출처