Tricarbonylbis 2-isocyano-l,3-dimethylbenzene iron

The same equipment is used as described in the procedure in Section B. The flask is charged with Fe(CO)4(CNC6H3Me2-l,3X1.79g, 6.0 mmol), CoCl2 2H20 (0.034 g, 0.2mmolX and toluene (30 mL), and the mixture is heated to 85°C with stirring. To the hot solution is added 2-isocyano-l,3-dimethylbenzene (1.57 g, 12.0 mmol). It is crucial to add the isocyanide to the hot solution. Otherwise, catalyst deactivation (believed to be due to isocyanide polymerization) occiurs. This results in a slu sh and incomplete 

The compounds Fe(CO), g(CNC4H3Me2-l,3X, (n = 1-5) are characterized by IR vibrational spectroscopy (vco and Vnc 1800-2200-on region) and by NM R spectroscopy (aromatic and methyl protons). Selected spectroscopic data for these complexes are given in the Table I. Infrared spectroscopy may conveniently be used for the monitoring of the progress of the substitution reaction, and NMR spectroscopy for an estimate of product purity. The complexes may also be characterized by mass spectrometry 

Gladkowski and F. R. Scholer, Abstracts of Papers from the Centennial American Chemical Society Meeting, New York, 1976, INOR 133. 

Shriver and M. A Drezdzon, The Manipulation of Air-Sensitive Compounds, 2nd ed, McGraw-Hill, New York, 1986. 

Perrin, W. L. F. Armaiego, and D. R. Perrin, Purification of Laboratory Chemictds, 2nd ed., Pergamon Press, Oxford, 1980. 

---