Preparation of Anhydrous CeCl3
Simple rapid heating of the hydrate alone may cause small amounts of hydrolysis. A useful form of anhydrous CeCl3 can be prepared if care is taken to heat the heptahydrate gradually to 140 °C (284 °F) over many hours under vacuum. This may or may not contain a little CeOCl from hydrolysis), but it is suitable for use with organolithium and Grignard reagents. Pure anhydrous CeCl3 can be made by dehydration of the hydrate either by slowly heating to 400 °C (752 °F) with 4-6 equivalents of ammonium chloride under high vacuum, or by heating with an excess of thionyl chloride for three hours. The anhydrous halide may alternatively be prepared from cerium metal and hydrogen chloride. It is usually purified by high temperature sublimation under high vacuum.
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