化学合成;制备:在温度0℃下,通过加料漏斗向含有三氯三聚氰和N,N-二异丙基乙胺(DIPEA)的四氢呋喃溶液中,小心地加入吗啉。将反应混合物在温度0℃下搅拌30min,然后真空浓缩。向残余物中加入乙酸乙酯(600mL),依次用水、0.5mol/L碳酸氢钠水溶液和盐水洗涤有机相。有机层用无水硫酸钠干燥,过滤并真空浓缩,通过硅胶柱色谱法(梯度洗脱氯仿/甲醇体积比=96/4-92/8-88/12)纯化,得到2,4-二氯-6-吗啉代-1,3,5-三嗪。
化学合成;医药中间体;农药中间体
路线1:
- 步骤:在5℃下向氰尿酸(230.5g,1,250mmol)的丙酮(2.25L)溶液中滴加吗啉(98.0g,1,125mmol)和三乙胺(113.0g,1,125mmol)的丙酮(2.25L)溶液。将所得混合物倒入水中。收集白色沉淀物并用甲醇洗涤,得到白色晶体2,4-二氯-6-吗啉代-1,3,5-三嗪(231.9g,986.9mmol),产率88%。
- 条件:With triethylamine In acetone at 5℃;
- 参考文献:[1] Patent: US2007/244110, 2007, A1. Location in patent: Page/Page column 4
路线2:
- 步骤:在-78℃下将氰尿酰氯(13.66g,74mmol)溶解在二氯甲烷(100mL)中,然后加入二异丙基乙胺(12.9mL,74mmol)。将反应混合物搅拌5分钟。在10分钟内将吗啉(6.46mL,74mmol)滴加到反应混合物中。过滤得到的白色沉淀,用水洗涤,干燥,得到定量收率的所需中间体(17g,100%)。
- 条件:With N-ethyl-N,N-diisopropylamine In dichloromethane at -78℃; for 0.17 h;
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