反応 #93784

ord-5761f7db8f3a4ee096a35db6e70f0979

反応条件

温度
44°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Reaction
  2. 2
    温度was heated up to 54.5° C. during addition (30 min)
  3. 3
    その他a violent exothermic reaction from 62° C. to 110° C
  4. 4
    その他16 min
  5. 5
    workup.DISTILLATIONVacuum distillation

実験手順

In a 50 ml apparatus, there were combined 7.7 g (0.1 mol) of allyl chloride and 0.05 ml of Pt catalyst solution. the mixture was heated to 44° C. and addition of a mixture of 11.6 g (0.1 mol) of Et3SiH and 1.4 g (0.01 mol) of Cl3SiH begun. Reaction was heated up to 54.5° C. during addition (30 min). There was a violent exothermic reaction from 62° C. to 110° C. 16 min later. Vacuum distillation yielded 7.79 g (40.5%) of Et3SiCH2CH2CH2Cl, with a Et3SiCH2CH2CH2Cl/Et3SiCl selectivity ratio of 1.23. This example and the previous one show that the preferred sequence of combination of reactants for most effective Cl3SiH promotion of the reaction of Et3SiH with allyl chloride is that of Example 24.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04614812uspto-grants-1986_09