Method for preparing carbonyls of ruthenium and osmium

Abstract

Abstract CARBONYLS OF THE FORMULA M3(CO)12, WHERE M IS RUTHENIUM OR OSIUM, ARE PREPARED BY REACTING A SOLUTION OF A HALIDE (SUCH AS A CHLORIDE, BROMIDE, OR IODIDE), A HALIDE DERIVATIVE, OR A CARBONYL HALIDE OF RUTHENIUM OR OSMIUM IN A FIRST SOLVENT WITH CARBON MONOXIDE AT A TEMPERATURE OF FROM ABOUT 100*C TO ABOUT 150*C. AT ATMOSPHERIC PRESSURE UNTIL A CARBONYL HALIDE COMPLEX IS FORMED. A SECOND SOLVENT IS THEN ADDED IN SUFFICIENT QUANTITY TO LOWER THE BOILING POINT OF THE RESULTANT SOLUTION TO LESS THAN 100*C. A QUANTITY OF ZINC IS ADDED AND THE SYSTEM IS REACTED WITH ADDITIONAL CARBON MONOXIDE AT A TEMPERATURE LESS THAN 100*C.UNTIL PRECIPITATION OF THE DESIRED DODECACARBONYL IS SUBSTANTIALLY COMPLETE. EACH OF THE TWO SOLVENTS SHOULD PREFERABLY HAVE THE FORLLOWING PROPERTIES. (1) ACT AS A SOLVENT FOR THE STARTING HALIDE OF RUTHENIUM OR OSMIUM; (2) NOT ENTER INTO THE REACTION; AND (3) NOT ACT AS A SOLVENT FOR THE DODECACARBONYL PRODUCT. IN ADDITION THE FIRST SOLVENT SHOULD BOIL AT A TEM BETWEEN 100*C. AND 150*C., AND THE SECOND SOLVENT SHOULD BOIL AT A TEMPERATURE OF LESS THAN 100*C.

Inventors

• 👤 J Dawes
• 👤 J Holmes

Bibliographic Details