A Lacunar Cyclidene Complex of Iron II

The methanol is removed by rotary evaporation at reduced pressure under a nitrogen atmosphere, and 50 to lOOmL of dry benzene (sodium dried) is added. 

The deacetylated Product VII is moisture sensitive and should not be exposed to the atmosphere. Analytical data are not normally obtained, and the intermediate is used immediately for the following step. The chemical and physical properties of the compound have been extensively studied. 

Ten grams (0.033 mol) of the deacetylated nickel(II) Complex VII, freshly prepared as described in Section B.l, is dissolved in 400mL of dry degassed 

A dark brown band remains on the column while the broad orange band is collected. The eluate is concentrated by rotary evaporation, and ethanol is added to induce precipitation of the product. The Product VIII is collected by suction filtration and dried in vacuo over P40,4. Yield 11.9g (70%). 

A 1-L one-necked round-bottomed flask containing a stirring bar is charged with 10.5 g (0.020 mol) of the product VIII from Section B.2, which has been dried in a vacuum oven overnight. A 2S0-mL volume of dry dichloromethane is added, giving a red solution. To this solution is added 10 g (0.06 mol) of methyl trifluoromethanesulfonate.  

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