Nitrido-bis triphenylphosphorus l Acetate

The procedure followed was first reported by Martinsen and Songstang and was performed with minor modifications. In a general preparation, 11.64g (0.02028 mol) of (PPN)C1 (Aldrich) is dissolved by heating in 120 mL of distilled and deionized water in a 250-mL Erlenmeyer flask. A 40-g quantity (0.4 mol) of potassium acetate in SO to 60 mL of water is added to the hot (PPN)C1 solution. The reaction mixture is stirred for 2 h and then placed in an ice bath for another hour. After filtration, the white solid is washed with cold water (3 x 1 mL) and then with cold diethyl ether (3x1 mL). The solid is 

Although an aqueous solution of this solid still gave a positive chloride ion test with AgNOs, the NMR aromatic-methyl integrations were 30 2.7, indicating less chloride ion contamination. A sample of (PPN) acetate was examined for chloride ion by elemental analysis (Galbraith) and it was determined to contain 3% (PPN)CI by weight. 

p-NITRIDO-BIS(TRIPHENYLPHOSPHORUS)(l +) PENTACARBONYL ACETATO GROUP 6 METAL 

All operations are carried out under nitrogen, with rigorous exclusion of air and moisture. Solvents are dried and deoxygenated by distillation from sodium benzophenone solution and collected under an N] atmosphere. 

The IR absorption bands for the three pentacarbonyl acetato compounds can be seen in Table II. Four bands are found in the CO stretching region, and two bands are attributed to the acetate moiety. The proton and C NMR resonance peaks are listed in Table III for this family of compounds. 

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