Azide aluminum

An ether solution of AIH3 is prepared from LiAlH and AICI3, and is then filtered and frozen in a liquid-nitrogen-cooled trap, (of. p. 807). An excess of anhydrous HN3 dissolved in ether is added, and the contents of the trap are allowed to melt slowly by gradually removing the Dewar flask. The evolution of l ydrogen starts at —116°C. The trap is then allowed to warm to room temperature vacuum is applied and the ether and excess HN3 are distilled off with renewed cooling. The product Al(Na)3 remains as a white powder. 

Very moisture sensitive. The compound may be shock detonated. Soluble in tetrahydrofuran. 

Very pure, finely divided aluminum powder (1.8 g.) and 2.9 g. of purified, dried red phosphorus are ground together in a mortar. 

A somewhat less pure product is obtained when a mixture of 27 g. of aluminum powder and 31 g. of red P is ignited with a burning magnesium strip (use safety goggles ) in an iron crucible. The crucible should not be more than half full, since the mass ejg)ands during the reaction and may overflow. In any case, the crucible should be covered with a lid. The yellowish to gray-black reaction mass is ground in a heated mortar. 

Yellowish-gray to dark, crystalline. Reacts with water to form PHg. Crystallizes in the zinc blende structure. 

---

Pyrolysis of diethyl aluminum azide [(C2H5)2A1N3] at 450-870°C). 

The pyrolysis of aluminum-nitrogen organic complexes, such as diethyl aluminum azide [(C2H5)2A1N3], is also used successfully at low deposition temperatures (450-870°C).0 l Another metallo-organic, hexakis(dimethylamido)dialuminum, reacting with ammonia allows deposition at 200-250°C at atmospheric pressure. 1... 

Aluminum Azide. See under Azides, Inorganic Alumtnu m Block (of Kreulen) is a hollow A1 block used for detg the tendency of coal and other materials to spontaneous combustion... 

Treatment of ethyl 2-(l-isoquinolylaminomethylene)cyanoacetate (238) with aluminum azide, prepared in situ from aluminum chloride and sodium azide, in boiling tetrahydrofuran gave 3-(l//-tetrazol-5-yl)-4//-pyrimido-[2,l-a]isoquinolin-4-one (239) (78USP4127720). The 8,9,10,11-tetrahydro derivative of compound 239 was similarly prepared (80USP4209620). 

Aluminum Azide A321-L Aluminum Carbide. See under Acetylides and Carbides A70-L Aluminum Triazide A521-L American Ammonium Nitrate Dynamites A355 (table)... 

With sterically hindered aldehydes and ketones considerably higher yields of (36) (68-86% vj. 8-32%) are obtained by the use of aluminum azide (35) instead of (34). 

Besides water and the carboxylic acids (3), hydrazoic acid (34) is the only acid that can be combined with carbonyl compounds (4) and isocyanides (5) to form a tetrazole derivative (37), a three-component adduct, in 7-95% yield.2 -32 With sterically hindered aldehydes and ketones considerably higher yields of (36) (68-86% vs. 8-32%) are obtained by the use of aluminum azide (35) instead of (34). ... 

A s3mthesis of 4-substituted 1,2,3-triazoles involves reaction of 1-alkynes with diorgano-aluminum azides. The inexpensive and nontoxic azide reagents are available from mixing R2AICI with NaN3 in toluene. ... 

---