Tetracarbonyl diethylamino methylidyne isocyanato tungsten

All operations are carried out under dry, oxygen-free nitrogen, using dry and nitrogen-saturated solvents. The silica gel (Merck) (0.06-0.20 mm) was held 5 h in vacuo and saturated with nitrogen. [Pg.42]

In a 100-mL round-bottomed flask equipped with N2 inlet, [W(CO)5(CNEt2)] [BF4] (2.1 g, 4.2 mmol) is added to 30 mL of dichloromethane at — 40 °C, followed by tetraethylammonium cyanate (1.5 g, 8.7 mmol) while stirring. After 30 min, the orange solution is taken directly to column chromatography1411 (silica gel, — 40 °C, column length 40 cm, width 3 cm). Elution with dichloromethane-diethyl ether (1 1) into a cooled (—40 °C) Schlenk tube with N2 inlet yields a dark orange solution, which is reduced in vacuo to 15mL. The product (0.95 g, 54%) is precipitated with 25 mL of pentane at — 40 °C and washed twice with 20 mL of cold pentane. [Pg.42]

For a survey see K. H. Dotz, H. Fischer, P. Hoffmann, F. R. Kreissl, U. Schubert and K. Weiss Transition Metal Carbene Complexes, Verlag Chemie, Weinheim, 1983, p, 176 [Pg.43]

Shriver, The Manipulation of Air-Sensitive Compounds, McGraw-Hill, New York, 1969. [Pg.43]

Fischer, U. Schubert, W. Kleine, and H. Fischer, Inorg. Synth. 19,168 (1979) (b) This compound is prepared like the homologous chromium complex (p. 168) (c) A description of the chromatography column is found on p. 166. [Pg.43]

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