化学合成。
化学合成
合成路线 1(1. 合成:83942-10-3)
产率:88.5%
合成条件:With trichlorophosphate In tolueneReflux
实验步骤:2)中间体4,5-二氯-6-甲基嘧啶的制备将50ml POCl 3滴加到14.5g(0.1mol)4-羟基-5-氯-6-甲基嘧啶在50mL甲苯中的溶液中, 加入后将混合物回流5-7小时。 通过薄层色谱监测反应结束后,将反应混合物减压浓缩除去甲苯和额外的POCl 3,然后倒入冰水中。 用乙酸乙酯(3×50ml)萃取水相,出现有机相,用无水硫酸镁干燥,过滤,然后减压浓缩。 通过二氧化硅柱纯化残余物,得到14.43g,为黄色液体,产率为88.5%。
参考文献:
- [1] Patent: US2015/225378, 2015, A1. Location in patent: Paragraph 0163; 0164 [2] Patent: EP2913325, 2015, A1. Location in patent: Paragraph 0453; 0454 [3] Patent: CN105348298, 2016, A. Location in patent: Paragraph 0421; 0422; 0423 [4] Patent: CN105732585, 2016, A. Location in patent: Paragraph 0371; 0372; 0373 [5] Patent: CN105777717, 2016, A. Location in patent: Paragraph 0360; 0361; 0362 [6] Patent: US2016/332991, 2016, A1. Location in patent: Paragraph 0364; 0365 [7] Patent: CN104292169, 2018, B. Location in patent: Paragraph 0460; 0461; 0462 [8] Patent: CN108059629, 2018, A. Location in patent: Paragraph 0267; 0271-0273 [9] Patent: US2018/141961, 2018, A1. Location in patent: Paragraph 0344; 0345 [10] Patent: CN107778298, 2018, A. Location in patent: Paragraph 0400; 0404; 0405; 0406 [11] Journal of Fluorine Chemistry, 2017, vol. 201, p. 49 - 54