反应详情

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

1. customwere prepared in a series of experiments
2. temperaturemaintained the reaction temperature (130°-140°)
3. additionWhen this addition
4. temperaturewas maintained at 130°-140° for several hours
5. customExcess BuBr was removed by distillation
6. temperatureAfter cooling to about 60°-80° the reaction liquor
7. customwas decanted from the tin
8. extractionextracted with 3 volumes of hydrocarbon (b.p. 145°-60°)
9. distillationthe hydrocarbon distilled