Sodium Hydroxide → HCID 178458744, compound

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Reaction Steps

124 g (0.8 mol) of 2-dimethylamino-4,6-dihydroxypyrimidine are stirred with 800 cc of 1N sodium hydroxide solution at 60° for 1 hour. 171 g (0.8 mol) of p-toluenesulphonic acid-n-propyl ester are added dropwise at 90° over the course of 1 hour and the pH is kept at 8-8.5 by the dropwise addition of 1N sodium hydroxide solution. The mixture is stirred at 90° for 16 hours, cooled to 5°, neutralized with glacial acetic acid and allowed to stand at room temperature for 6 hours. The precipitated crystals are subsequently filtered by suction, washed with water, dissolved in approximately 700 cc of chloroform, dried over sodium sulphate and evaporated to dryness in a vacuum. The residue is decomposed with 500 cc of petroleum ether, filtered by suction and recrystallized from benzene, washed with petroleum ether and dried at 60° in a high vacuum. M.P.: 194°-195°.

Provenance & Evidence