Mechanochemical synthesis of an organometallic compound: a high volume manufacturing method

Faraday Discuss. 2014:170:83-91. doi: 10.1039/c3fd00157a.

Abstract

Chemical vapor deposition (CVD) precursor chemicals are held to some of the highest purity levels in industry. Many metal reagents form stable, unbreakable adducts with the coordinating solvents that are necessary for solvating highly polar reagents. These adducts are undesirable and must be removed prior to usage. Herein we describe a mechanochemical approach to the synthesis of bis(n-propyltetramethylcyclopentadienyl)strontium that eliminates the use of strongly coordinating solvents. This method overcomes the solubility problems of the two reagents without the formation of stable, unbreakable adducts. We utilize a unique reactor geometry that facilitates mechanochemical syntheses while simplifying handling and allowing for "one pot" production. The synthesis was scaled to five hundred gram lot sizes in a six liter reactor. This technique is applicable to many syntheses and is linearly scalable - limited only by reactor size.