Three new methods for large scale synthesis of electronic grade trimethylgallium and trimethylindium are presented. These methods are based on direct synthesis of trialkylgallium compounds from the Ga/Mg alloy or the mixture of this metals and alkyl halides, RX. The first method consists in the cleavage of the stable trimethylgallium-diethyl ether adduct by heating it in the mixture with ether of higher boiling point. The second one is the reaction of the mixture of Ga and Mg with methyl iodide in a high boiling ether solvent such as diisoamyl ether, i-Am₂O. The third method consist in preliminary formation of the stable adducts of trimethylgallium or trimethylindium and alkali metal fluorides from their etherates, followed by removing ethers and thermal decomposition of adducts to yield free trimethylgallium or trimethylindium respectively.