Abstract: | The reaction of the Si8O208? silicate anion with X(CH3)2SiCl (X?H or CH3) has been studied to develop a cost‐effective procedure for synthesizing Si8O20Si(CH3)2X]8 in high yield. Use of hexane as solvent and adjustment of the reaction temperature to ca 20 °C were found to be effective in promoting the reaction, by which Si8O20Si(CH3)2X]8 could be produced in good yield employing 24 mol of X(CH3)2SiCl per mole of Si8O208?. It was also demonstrated that the yield of Si8O20Si(CH3)2X]8 depends on the amount of solvent, suggesting that the amount is an important factor when scaling up the reaction to produce a large quantity of Si8O20Si(CH3)2X]8. Copyright © 2003 John Wiley & Sons, Ltd. |