90213-67-5
90213-67-5 结构式
基本信息
2,4-二氯-7-甲基-7H-吡咯并[2,3-D]嘧啶
2,4-Dichlor-7-methyl-7H-pyrrolo[2,3-d]pyrimidin
2,4-dichloro-7-Methyl-7H-pyrrolo[2,3-d]pyriMidine
7H-Pyrrolo[2,3-d]pyrimidine, 2,4-dichloro-7-methyl-
制备方法
90213-66-4
74-88-4
90213-67-5
向氢化钠(480 mg,12.00 mmol,1.10当量,60%分散于矿物油中)的四氢呋喃(50 mL)悬浮液中,缓慢滴加2,4-二氯-7H-吡咯并[2,3-d]嘧啶(2 g,10.64 mmol,1.00当量)的四氢呋喃(50 mL)溶液。反应混合物在0℃下搅拌30分钟后,于相同温度下逐滴加入碘甲烷(1.66 g,11.70 mmol,1.10当量)。加毕,将反应体系升至室温并搅拌过夜。反应完成后,向混合物中加入水(20 mL)淬灭反应,随后用乙酸乙酯萃取。合并的有机相用饱和食盐水洗涤,无水硫酸钠干燥,过滤后减压浓缩。粗产物通过硅胶柱色谱纯化,以乙酸乙酯/石油醚(1:5,v/v)为洗脱剂,得到2.1 g(收率98%)标题化合物2,4-二氯-7-甲基-7H-吡咯并[2,3-d]嘧啶,为白色固体。LC-MS(ESI, m/z):202 [M+H]+。
参考文献:
[1] Patent: US2015/57260, 2015, A1. Location in patent: Paragraph 0436; 0437; 0588; 0589
[2] Patent: WO2015/25026, 2015, A1. Location in patent: Page/Page column 118
[3] Patent: WO2017/59191, 2017, A1. Location in patent: Paragraph 00235-00239
[4] Patent: WO2017/46739, 2017, A1. Location in patent: Page/Page column 51
[5] Patent: CN107226808, 2017, A. Location in patent: Paragraph 0366-0369