Thermally stable dialkylantimony(V) compounds of the type R2SbX3 (X= OMe, OEt, or OAc) have been prepared in good yields and purity. Hydrolysis of the trialkoxodialkylantimony compounds, R2Sb(OR′)3, results in the quantitative formation of hydroxo(oxo)dialkylantimony compounds, R2Sb(O)OH. These compounds are thermally stable and not sensitive towards oxygen in the air. Therefore, they form suitable