Methanol → A-Link 15

참여 물질

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반응 단계

A one-liter three-neck round bottom flask was equipped with a magnetic stir bar, standard heating mantle, thermocouple, addition funnel, condenser and N2 inlet/bubbler. The flask was charged with 220 g (1.80 mols) of trimethoxysilane and heated to 60° C. at which temperature 0.25 ml of platinum tris(divinyltetramethyl disiloxane)diplatinum (0) (5% Pt content in toluene—referred to as Pt catalyst throughout these examples) was added. The solution was further heated to 68° C. and dropwise addition of 150 g (1.52 mols) of N-ethylmethallylamine was then conducted over a period of 45 minutes. After addition, the contents were heated to 90° C. and maintained at this temperature for 1 hr. The temperature was then increased to 105° C. and held for 4.5 hrs. Upon completion of the reaction, the mixture was cooled to room temperature and 16 g (0.5 mols) of methanol were added and gently heated prior to distillation. Final purification via vacuum distillation yielded 273 g (1.24 mols) of N-ethyl-3-trimethoxysilyl-2-methylpropanamine. The product (b.p. 98-100° C. at 12 mm Hg) was characterized via GC/MS. The isolated yield was 82%. Product structure was supported by GC/MS analysis.

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