反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a round bottom flask equipped with a magnetic stir bar was added N-(4-fluorophenyl)-N′-(4-{[1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazolo[3,4-d]pyrimidin-4-yl]oxy}phenyl)cyclopropane-1,1-dicarboxamide (0.050 mg, 0.10 mmol, 1.0 eq.) and 4M HCl/Dioxane (5 ml). After 5 minutes ether was added. The resulting solid was filtered and washed twice with ether. The solid was further dried under vacuum to give N-(4-fluorophenyl)-N′-[4-(1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)phenyl]cyclopropane-1,1-dicarboxamide (0.027 g, 67% yield). 1H NMR (400 MHz, DMSO): 10.20 (s, 1H), 10.10 (s, 1H), 8.50 (s, 1H), 8.06 (s, 1H), 7.75 (m, 2H), 7.67 (m, 2H), 7.27 (m, 2H), 7.13 (m, 2H), 4.47 (bs, 1H), 1.47 (s, 4H); MS (ESI) for C22H17FN6O3: 433 (MH+).
WORKUP
后处理
- customTo a round bottom flask equipped with a magnetic stir bar
- filtrationThe resulting solid was filtered
- washwashed twice with ether
- customThe solid was further dried under vacuum