50 ml of 98 tripropylamine and 1 l of 99 i proh and cooled to u2212 78 u00b0 c in a dry ice isopropanol bath to this mixture solutions of 45 0 g 40 aqueous glyoxal 0 310 mole diluted to 250 ml with isopropanol and 30 0 g 0 205 moles of 96 tren diluted to 250 ml were simultaneously added over a period of 2 hrs with vigorous stirring initial concentration of glyoxal 1 24 m initial concentration of tren 0 82 m then the reaction mixture was allowed to warm up overnight and briefly warmed up to 60 u00b0 c to ensure that the formation of compound 2 was complete it was cooled to room temperature while nitrogen gas was blown over its surface on the next day the remaining solution its volume had decreased to u02dc 500 ml as a result of a partial solvent evaporation was cooled down to u2212 78 u00b0 c sodium metal 49 g 2 13 mole cut into six roughly equal pieces was added to the solution with gentle stirring in a nitrogen atmosphere gaseous nh 3 was then bubbled into the solution until the volume of the liquid increased by u02dc 500 ml at this point small drops of na u2014 nh 3 golden liquid phase surrounded by thin blue diffusion layers started to float.