6601-22-5 2,4-二氯-6-吗啉代-1,3,5-三嗪

干冰运输相关信息：危险性质为非危险化学品，海关编码为2934.99.4400。

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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