The current methods for the preparation of ethyl orthosilicate do not give satisfactory results. It is found that the low yield is due to the use of excess alcohol, which, in presence of hydrogen chloride, produces water and causes the ethyl orthosilicate to undergo a hydrolytic polycondensation. The condensation products have been isolated and identified as 1,3-hexaethoxydisiloxane and 1,3,5-octaethoxytrisiloxane. An improved method,consisting of the addition of equivalent quantities of silicon tetrachloride and anhydrous ethyl alcohol into ice-cold ethyl orthosilicate as diluent,is recommended. The reaction mixture gives 95% of theoretical yield of the ethyl orthosilicate.