Patent GB-986522-A (GB)
Title: Process for the manufacture of complex alkali-organo compounds of aluminium or boron
IPC: C07F5/06
Filed: 1962-04-30
Abstract: Complex alkali organo compounds of aluminium and of boron of formula MZRm(OR1)n, where M signifies sodium or potassium, Z aluminium or boron, R an alkyl radical, R1 an alkyl, cycloalkyl or aryl radical which may be substituted, m and n are preferably whole numbers from 1 to 3, m+n being equal to 4, are prepared by reacting compounds of formula ZRx(OR1)y, where Z, R and R1 are as above, x is preferably a whole number from 0 to 2 and y is preferably a whole number from 1 to 3, x+y being equal to 3, with alkyl halides and sodium or potassium. The R radicals may be the same or different and in particular C1- 10 straight chain primary alkyl radicals:  the R1 radicals are preferably C1- 10 alkyl or cycloalkyl radicals.  The sodium or potassium is preferably introduced in finely divided form, the reaction being carried out at temperatures below 100 DEG  C. A diluent or solvent may be employed, e.g. an aromatic hydrocarbon or in some cases an aliphatic or olefinic hydrocarbon, straight chain or cyclic ethers, e.g. tetrahydrofuran, dioxane, diethyl ether, dibutyl ether and polyethers (ethylene glycol dialkyl ether), or tertiary amines, e.g. trimethylamine and dimethyl aniline.  A modification of the process yields sodium tetra-alkyl aluminium compounds:  the reaction between sodium and the alkyl halide is in this case carried out in the presence of a trialkyl aluminium compound.  It is preferred to treat the sodium with a little alkyl halide before addition of the trialkyl aluminium.  A dialkyl aluminium monoalkoxide may also be used as initiator.  In a further modification a layer of liquid sodium amalgam as anode may be covered with one of the complex compounds of the invention dissolved if desired in tetrahydrofurun or other solvent.  A wire netting cathode is laid over the amalgam and the reaction components gradually stirred in with simultaneous electrolysis, thus producing more and more of the desired compounds. In another form of the invention alkyl radicals may be introduced into boric acid esters by converting the boric acid esters into the complexes of the invention, which in turn are converted into monoalkyl boric acids by dilute acids which can then be esterified and renewed "alkylation" according to the invention into dialkyl boric acids and finally into trialkyl boron compounds. Specification 955,252 is referred to.ALSO:Complex alkali-organo compounds of aluminium of formula MZRm(OR1)n where M is sodium or potassium, Z aluminium, R an alkyl radical, R1 an alkyl, cycloalkyl or aryl radical which may be substituted, m and n are preferably whole numbers from 1 to 3, m+n being equal to 4, may be prepared by covering a layer of liquid sodium amalgam as anode with one of the complexes of the invention, if desired in tetrahydrofuran or other solvent.  A wire netting cathode is laid over the amalgam and an alkyl halide and a compound of formula ZRx(OR1)y where Z, R and R1 are as above, x is preferably a whole number from 0 to 2, y is preferably a whole number from 1 to 3 and x+y is equal to 3, are gradually stirred in with simultaneous electrolysis, thus producing more of the desired complex.  Specification 955,252 is referred to.