Highly pure tri:aryl-borane cpds. prodn. by reproducible process - by reacting boron tri:halide in inert solvent with slight excess of aryl magnesium halide in linear ether and removing ether and magnesium salt
摘要
Prepn. of highly pure triarylborane (I) in high yield by reacting B tri-halide (II) with aryl Mg halide (III) comprises: 1) reacting 1 mole (II), as 0.1-8.0 M soln. in an inert solvent (IV) with 3.1-3.5 mole (III) as 0,1-3.0 M soln. in a linear ether solvent (V); (2) distilling off (V) to promote further reaction of the mixt.; and then 3) crystallising the halogenated Mg salt (VI) formed as by-prod. to increase the (I) recovery ratio. Pref. on crystallisation of (VI), (I) included in (VI) is released by distilling (V) from the reaction mixt. ADVANTAGE - The process is stable and gives as reproducible results as possible in (I) prodn. on the technical scale.