Aluminum chloride is removed effectively from compound mixtures containing organochlorosilanes such as are produced in the direct synthesis, by adding a diluent containing organochlorosilanes and optionally chloromethane to a solids content <15% and a concentration of compounds having a boiling point >71.degree. C. of less than 25%, and evaporating this diluted mixture into a volatile product stream and an AlCl.sub.3-containing solid.