Ethoxycarbonyl methylidyne-tris tricarbonylcobalt

three-necked, round-bottomed flask is equipped with a serum cap, a nitrogen inlet tube connected to a T-piece that leads to a prepurified nitrogen supply and to a Nujol bubbler, and a solids-transfer tube (in the center neck). The flask is evacuated, flamed out, and flushed with dry nitrogen. It then is charged with octacarbonyldicobalt (73.4 g, 0.215 mole) and 440 mL of dry tetrahydrofuran (THF). The transfer tube is removed and replaced with an 

The mixture is allowed to cool to room temperature and then is suction filtered in air to obtain a bright-blue residue (cobalt salts, which are discarded) and an intensely purple-colored filtrate. The latter is treated with 1500 mL of 10% aqueous hydrochloric acid to destroy remaining noncluster cobalt carbonyl. The product ester is extracted into 500 mL of pentane. The extracts are washed several times with equal portions of water. The organic layer is dried over anhydrous magnesium sulfate. Filtration is followed by evaporation of the filtrate at reduced pressure (rotary evaporator). The solid that remains is sublimed at 50° and 0.1 torr to yield 38.79 g (53%) of purple crystals of /j3-[(ethoxycar-bonyl)methylidyne]-tris(tricarbonylcobalt), mp 45-46°,2 Anal. Calcd. for CuHjOuCoj C, 30.38 H, 0.98. Found C, 30.30 H, 0.96. 

ju3- [(METHYLAMINO)CARBONYL]METHYLIDYNE -TRIS (TRIC ARBONYLCOBALT) 

The apparatus is equipped with a magnetic stirring bar, dried, flushed with nitrogen and charged with 1.04 g (2.0 mmole) of /i3 - [(ethoxycarbonyl)-methylidyne]-tris(tricarbonylcobalt) and 15 mL of propionic anhydride. The mixture is stirred under nitrogen (apparatus horizontal) until the cobalt complex 

jli3-(CHLOROMETHYLIDYNE)- AND ti3-[(ferf-BUTOXYCARBONYL)METHYLIDYNE] -TRIS (TRICARBONYLCOBALT) 

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M3-[(ETHOXYCARBONYL)METHYLIDYNE] - and JU3- [(METHYLAMINO)CARBONYL] METHYLIDYNE -TRIS (TRICARBONYLCOBALT)... 

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