Tetraphosphorus Hexamethylhexaimide

TETRAPHOSPHORUS HEXAMETHYLHEXAIMIDE [2,4,6,8,9,10-Hexamethyl-2,4,6,8,9,10-hexaaza-l,3,6,7-tetraphosphaadamantane Phosphorus (III) Methylimide] 

Tetraphosphorus hexamethylhexaimide, P4N6(CHs) , represents the first isolated memberof a class of phosphorus- 

With nitrogen flowing at a very slow rate but at a slightly greater pressure than for the flow of methylamine, 64,6 ml. (1.60 mols) of anhydrous tank methylamine (to the mark 

The phosphorus(III) chloride is added dropwise during a one-hour period, with occasional stirring. The resulting yellow solid and clear liquid are allowed to stand overnight at —78 and then to warm slowly over a 2-day period to —30°. Above —30° a rock salt-ice mixture is used to maintain the bath temperature. At this stage of the procedure a yellow-white solid is present in the excess amine. Over the next 2 days the temperature is allowed to rise slowly to room temperature, during which time the solution becomes yellow and viscous. The reaction product is then warmed to 50° and maintained at that temperature for about 4 hours to drive off the excess amine and until a white solid remains. The kettle and product are then placed in a nitrogen-filled dry-box. 

Tetraphosphorus hexamethylhexaimide is a moisture-sensitive, white crystalline solid melting at 122 to 123° and boiling at 303 to 304° at 737 mm. It is soluble in a wide variety of organic solvents, including benzene, toluene, n-hexane, diethyl ether, acetone, and carbon tetrachloride. It is insoluble in water but dissolves slowly in a hot aqueous aiumonia solution. 

6° per minute) shows no phase change but rather a browning which begins at 204° and becomes complete at 234°. Gas evolution is noted at 145°. A simultaneous differential thermogram-gas profile shows an endotherm with gas evolution at 190° and an exotherm with marked gas evolution at 210°. The azido groups show strong characteristic absorptions in the infrared. 

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Phenyllead(IV) azides, synthesis 15 Tetraphosphorus hexamethylhexaimide, synthesis 16 Diphenyl phosphorochloridite, synthesis 17 Diphenylphosphinic acid, synthesis 18 (2,2-Dimethylhydrazino)diphenylphosphine, synthesis 19 Alkoxy- and aryloxycyclophosphazenes, synthesis 20 Mercapto derivatives of chlorocyclophosphazencs, synthesis 21 Dialkylsulfamoyl chlorides, synthesis 27 N- and J T,A1 -Substituted sulfamides, synthesis 28 Dialkylamides of (trichlorophosphoranylidene)sulfamic acid, synthesis 29... 

Tetraphosphorus hexamethylhexaimide reacts with oxygen at 170° to give P202(NCH3)3. With boron fluoride and boron chloride, a variety of substances are formed A water-soluble white solid adduct, P4N6(CH3)7l, forms with methyl iodide. The following reaction proceeds almost quantitatively at —78° ... 

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