반응 #93782
ord-e63054bf8700455e8d36e41abd7c4600
반응 조건
후처리
- 1온도Heat
- 2기타was applied to 60° C.
- 3기타a smooth exothermic reaction up to 80° C.
- 4workup.ADDITIONby the end of the addition (15 min) with temperature
- 5기타to rise to 129° C
- 6기타5 min
- 7workup.DISTILLATIONVacuum distillation
실험 절차
In a 25 ml apparatus, there were combined 11.6 g (0.1 mol) of Et3SiH and 0.05 ml of Pt catalyst solution. Heat was applied to 60° C. and addition of a mixture of 7.7 g (0.1 mol) of allyl chloride and 1.4 g (0.01 mol) of Cl3SiH begun. There was a smooth exothermic reaction up to 80° C. by the end of the addition (15 min) with temperature continuing to rise to 129° C. 5 min later. Vacuum distillation yielded 12.12 g (63.0%) of Et3SiCH2CH2CH2Cl, with a Et3SiCH2CH2CH2Cl/Et3SiCl molar ratio of 2.73. This example shows that low levels of Cl3SiH effectively promote both rate and yield of the reaction between Et3SiH and allyl chloride, particularly when the low levels are maintained throughout the reaction by replenishment.