反应详情

In accordance with one variation of the method of the present invention, two moles of n-butylchloride and two moles of activated magnesium are reacted in a liquid hydrocarbon solvent having a boiling point equal to or less than 100° C. to produce a di-n-butylmagnesium plus magnesium chloride product which may be a complex, and which precipitates. In the second step the di-n-butylmagnesium-magnesium chloride complex is reacted with two moles of diisopropylamine (DIPA) to yield two moles of chloromagnesium amide plus two moles of butane which leaves as a gas; this solid product may be a complex of magnesium bisdiisopropylamide and magnesium chloride. Chloromagnesium amide complex as a solid is also prepared in one step reaction by reacting activated magnesium metal with one mole of n-butyl chloride and one mole of diisopropylamine in hydrocarbon solvents such as hexane, cyclohexane, or heptane. The chloromagnesium amide or the complex product of the previous step is reacted with normal n-butyllithium to produce soluble n-butylmagnesiumamide plus solid lithium chloride. The major reaction product is a magnesium bisdiisopropylamide complexed with di-n-butylmagnesium. This product is also identified as n-butylmagnesium diisopropylamide (n-BuMgN(iPr)2); in the next step this reaction product is reacted with additional diisopropylamine to produce the magnesium bisdiisopropylamide product plus butane. This product is soluble so the lithium chloride can be removed by filtration. Should a lower boiling hydrocarbon be desired in the process, then diisopropylamine is advantageously added at the same time as the n-butylchloride in step 1 to lower the reaction temperature. It is thought that the diisopropylamine acts as a Lewis base in this reaction as well as a reactant. In like manner, diisopropylamine and n-butyllithium can also be added simultaneously to the chloromagnesium(organo)amide in step 3 to form magnesium bisdiisopropylamide.

1. customless than 100° C.