solution was cooled down to u2212 78 u00b0 c again and sodium metal 49 g 2 13 mole cut into 1 g pieces was added to the solution upon gentle stirring after that gaseous nh3 was blown into the solution till the volume of the liquid increased by u02dc 500 ml by that time small drops of na nh 3 golden liquid phase surrounded by thin blue diffusion layers started to float to the surface the ammonia addition was then stopped the solution was vigorously stirred for 10 minutes and then it was allowed to warm up to room temperature overnight by the time the reaction mixture warmed up to room temperature ammonia was virtually gone and no na metal was left the obtained white slurry was poured into 2 l separation funnel 300 ml toluene and 200 ml h 2 o were added to it the whole flask was stirred and allowed to stand for an hour when the phases separated the lower phase containing concentrated solution of naoh was separated the rest of the solution was evaporated under vacuum at 100 u00b0 c and when the resulting viscous liquid was allowed to cool down to room temperature it yielded solid impure compound 1 that compound 1 was recrystallized from 100 ml h 2 o to give 20 0 g h 6 aza222 4h 2 o that was filtered at 0 u00b0 c and dried on filter the composition of the hydrate was deduced from the results of chn analyses yield of 1 4h 2 o 20 0 g 64 5 1 h nmr cdcl 3 containing d 2 o 2 477 ppm t j.