Example 2
To a 500 ml, flask fitted with a heating mantle, thermocouple, temperature controller, agitator and condenser, was added 1,4-DFDK (20.3 g) and sulfolane (112 g=100 mL). The mixture was heated, with agitation, to 150° C. The heat was turned off to allow the solution to cool just slightly, the solution was filtered through Whatman GF/F glass fiber filter pad in a pre-heated (125° C.) ceramic Büchner funnel into a clean 500 mL 3-neck flask. The initial flask was rinsed with hot sulfolane (38 g=30 mL) through the filter. The resulting filtered solution was reheated to redissolve the solids. The heating was discontinued and the solution allowed to cool at approximately 0.3° C./min to room temperature. The recrystallized solids were isolated by filtration in a Buchner funnel with a Whatman #4 filter paper. Air was pulled through the cake until no more solvent was seen dripping from the funnel. The solids were then transferred back to the 500 mL flask, Water and ethanol was added (250 mL of 90:10) and the slurry was agitated for 5 minutes and isolated by filtration in a Buchner funnel with a fresh Whatman #4 filter paper. The solids were transferred to an aluminum pan and vacuum oven dried at 130° C. and 27″ Hg for 24 h. The solids were allowed to cool to room temperature and transferred to a tared jar to afford 18.0 g (90%).
Analysis of the product is shown in Table 1