反应详情

温度

-5 °C

A solution of 2,4-diamino-6-methyl pyrimidine (1.0 gm) in water (60 ml) was cooled to 0° C in ice-salt bath and stirred mechanically. p-Iodo aniline (1.84 gm) was dissolved in ethanol (30 ml) and to this solution 3 N HCl (30 ml) was added. The solution was then cooled to -5° C. A solution of sodium nitrite (0.567 gm) in water (5 ml) was also cooled to 0° C. The sodium nitrite solution was then added to the p-iodo aniline solution. After shaking thoroughly, excess sodium nitrite was decomposed with a pinch of urea. The diazotized p-iodo aniline was then added to the pyrimidine solution. After stirring for ten minutes, the pH of the combined solution was adjusted to 7.0 with 30 percent sodium hydroxide. A precipitate appeared. After stirring two hours more, the product was filtered, dried in vacuum desiccator, and crystallized from ethanol. M.P. 243°-44° C. Yield: 2.5 gm (90 percent).

1. additionwas added
2. stirringAfter shaking thoroughly
3. stirringAfter stirring for ten minutes
4. stirringAfter stirring two hours more
5. filtrationthe product was filtered
6. customdried in vacuum desiccator
7. customcrystallized from ethanol