Organic Lab Reactions 301

Organic Lab Reactions 301 - 296 THE AROMATIC PRIMARY AMINO...

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296 THE AROMATIC PRIMARY AMINO GROUP solution in about five minutes; copious evolution of nitrogen occurs. After being stirred at ice temperature for two hours, the mixture is kept in an ice chest for about twenty hours and the yellow precipitate is then isolated- by nitration. The filtrate is extracted with ether, and, after addition of the yellow solid, the ether solution is washed twice with 50-cc. portions joi a. 10% sodium hydroxide^ solution, then dried over sodium sulfate, and the solvent is removed. The crystalline product weighs 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. 83 With 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°; efficient stirring is instituted, and 5.2 cc. (0.05 mole) of 50% hypophosphorous acid (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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