296 THE AROMATIC PRIMARY AMINO GROUPsolution in about five minutes; copious evolution of nitrogen occurs.After being stirred at ice temperature for two hours, the mixture is keptin an ice chest for about twenty hours and the yellow precipitate is thenisolated- by nitration. The filtrate is extracted with ether, and, afteraddition of the yellow solid, the ether solution is washed twice with50-cc.portionsjoi a.10% sodium hydroxide^ solution, then dried oversodium sulfate, and the solvent is removed. The crystalline productweighs 4.5 g. (90%); m.p. 92-93°. After one recrystallization from aque-ous ethanol (charcoal), there is obtained 4.25 g. (85%) of white needles;m.p.94.8-95.8°.1,3,5-Trinitrobenzene from 2,4,6-Trinitroaniline.83With gentle stir-ring, 2 g. (0.028 mole) of sodium nitrite is added to 55 cc. of sulfurlc acid(sp.gr.1.84).The resulting solution is cooled to —5° to 0°; efficientstirring is instituted, and 5.2 cc. (0.05 mole) of 50% hypophosphorousacid (precooled to —5° to 0°) is added rapidly. While a temperature of—5° to 0° is being maintained, a solution of 2.3 g. (0.01 mole) of 2,4,6-
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