Tributylamine → Bu3SnBr Bu2SnBr2

Beteiligte Stoffe

Reaktionsschritte

Crude tributyltin bromide (Bu3SnBr) containing up to 28% dibutyltin dibromide (Bu2SnBr2), and halogenotin by-product were prepared in a series of experiments, A-G. These involved heating tributylamine (Bu3N) with excess elemental tin and adding butyl bromide (BuBr) at a rate such that the reaction temperature of 130°-140°. was maintained. When this addition was complete, the reaction mass was maintained at 130°-140° for several hours more. Excess BuBr was then removed by distillation. After cooling to about 60°-80° the reaction liquor was decanted from the unreacted tin and extracted with 3 volumes of hydrocarbon spirits (b.p 145°-160°). The extracts were combined and the hydrocarbon distilled off leaving the crude Bu3SnBr-Bu2SnBr2 mixture. The halogenotin complex by-product remaining after the extraction was heated under vacuum to remove any residual hydrocarbon extractment and the product stored in plastic containers. The amounts of materials used and the products obtained are shown in table III.

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