化学合成。
医药
合成路线 1(1. 合成:5177-27-5)
产率:80%
合成条件:Stage #1: for 14 h; Stage #2: With sodium carbonate In water; ethyl acetate
实验步骤:将2.4-二氯-5-硝基 - 嘧啶(1.0当量)和铁(6.0当量)在乙酸中的浓度为0.4M的非均相溶液剧烈搅拌14小时。然后将混合物通过硅藻土。 用MeOH洗脱,真空除去挥发物,将残余物溶于EtOAc,用Na 2 CO 3(饱和),NaCl(饱和)洗涤,用MgSO 4干燥,过滤,真空除去挥发物。 2,4-二氯嘧啶-5-胺(80%)。 LCMS(m / z):157.0(MH +); LC Rt = 1.85分钟。
参考文献:
- [1] Patent: US2011/195980, 2011, A1. Location in patent: Page/Page column 17 [2] Patent: WO2011/106168, 2011, A1. Location in patent: Page/Page column 83; 84; 101; 102 [3] Journal of the Chemical Society, 1951, p. 1565,1568 [4] Journal of the Chemical Society, 1953, p. 1646 [5] Chemical and Pharmaceutical Bulletin, 1958, vol. 6, p. 352,354 [6] Patent: CN103864792, 2017, B. Location in patent: Paragraph 0357; 0358; 0359; 0360