Into a 250-mL round-bottomed flask prepare a solution of 0.66 g of sodium hydroxide and 5.0 g of 1,3,5-trimethoxy-2,4,6-trinitrobenzene in 100 mL of methyl alcohol.  Reflux this solution at 60 C for 24 hours.  Increase the heat to distill off the liquid and isolate the crystalline residue.  Add 30 mL of ether to the flask, filter to collect the insoluble material, and allow it to dry.  The material is sodium
3,5-dimethoxy-2,4,6-trinitrophenolate.

Place the crystals in a metal pressure container or a steel pipe.  Add 50 mL of anhydrous liquid ammonia to the vessel and seal it.  Allow the container to warm to room temperature at which time the pressure increases.  After 24 hours the container is opened and the ammonia is allowed to escape.  Wash out the container with 50 mL of toluene and collect the crystals on a filter.  Wash the crystals with an additional 25 mL of toluene and allow them to dry.  This material is a mixture of sodium and ammonium salts of 3,5-diamino-2,4,6-trinitrophenolate.

Into a beaker containing 500 mL of 3M hydrochloric acid add the dried crystals.  Stir this mixture for 24 hours.  Filter to collect the product, wash it thoroughly with water until no longer acidic, and allow to dry.  Place the crystals in the pressure vessel again and add 25 mL of anhydrous liquid ammonia.  Seal the vessel and let it sit at room temperature for 30 minutes.  Unseal the vessel and add 50 mL of toluene while the ammonia boils off.  Filter to collect the solid material, wash it with 25 mL of toluene, and allow to dry.  Final yield of pure ADAP is over 4 g or 93%.

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