Slight modifications, apported in the synthesis of (CH3)2AsX (X = Cl, Br) (I, II) by the reduction of cacodylic acid by underfosforic acid, are reported.
(CH3)2AsI (III) was prepared in a high purity state.
An improved method is given for the preparation of CH3AsCl2 (IV) and the yield is raised from 55 to 70%.
CH3AsBr2 (V) up to now unknown, was prepared by a method analogous to that for (IV). In (CH3)2 (VI) was prepared by the action of Hg(CH3)2 on In; with high‐purity Hg(CH3)2 it is necessary to add traces of I2 and Mg together with HgCl2, as catalysts; reaction starts within two hours.
We succeeded the synthesis of [(CH3)2AlX]2 (X = Cl, Br, I) (VII, VIII, IX) and of [CH3AlX2]2 (X = Cl, Br) (X, XI) in an all‐glass apparatus under atmospheric pressure; decantation of the sesquihalogenides from the slurry of unreacted Al was avoided.