By L. Brandsma, S.F. Vasilevsky, H.D. Verkruijsse
Homogeneous catalysis is a crucial method for the synthesis of high-valued chemical substances. L. Brandsma has rigorously chosen and checked the experimental systems illustrating the catalytic use of copper, nickel, and palladium compounds in natural synthesis. All tactics are on a preparative scale, make fiscal use of solvents and catalysts, keep away from poisonous components and feature excessive yields.
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Extra resources for Application of Transition Metal Catalysts in Organic Synthesis (Springer Laboratory)
The compound should be stored in the refrigerator. 15 2-lodo-1-methylimidazole THF + n-BuLi -70 cc .. 10 molar (n-BuLi). Apparatus: 1-1 round-bottomed, three-necked flask, equipped with a nitrogen inletthermometer combination, an efficient mechanical stirrer and an outlet; during the addition of iodine the outlet was replaced with a powder funnel. 10 mol of n-butyllithiurn in 64 ml of hexane was added over a few min by syringe, while keeping the temperature of the solution at --70°C by occasional cooling in a bath with liquid nitrogen.
Hexane:. 20 ~ 50 cC 12 Q ----. 2 Aryl and Hetaryl Halides Apparatus: 1-1 round-bottomed, three-necked flask equipped with a nitrogen inletthermometer combination, an efficient mechanical stirrer and a reflux condenser; for the iodination the condenser was replaced with a combination of dropping funnel and outlet. 30 mol of n-butyllithium in 192 ml of hexane was placed in the flask. 30 mol, 35 g) was added over a few sec through the condenser. 9 g) of freshly distilled I-methylpyrrole. The temperature of the mixture rose to about 50 °C and was kept at that level for an additional half hour.
This consists mainly of diethyl ether and can be removed by warming and temporarily passing a fast stream of nitrogen (or dry air) through the flask. The oily, grey solution is decanted from the excess of metal into another flask and weighed. 50 mol of MgBr2' Since the etherate does not crystallize out during storage at room temperature, the amount needed for some reaction can be determined by weighing. Regular greasing of the stopper of the storage flask is desired. Lithium-zinc exchange reactions (RLi + ZnCl 2 -+ RZnCI + LiCl) also proceed very smoothly.