반응 #93784

ord-5761f7db8f3a4ee096a35db6e70f0979

반응 조건

온도
44°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Reaction
  2. 2
    온도was heated up to 54.5° C. during addition (30 min)
  3. 3
    기타a violent exothermic reaction from 62° C. to 110° C
  4. 4
    기타16 min
  5. 5
    workup.DISTILLATIONVacuum distillation

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04614812uspto-grants-1986_09