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 3-({1-[(6-amino-1H-pyrazolo[3,4-b]pyridin-3-yl)methyl]-5-chloro-1H-indazol-4-yl}oxy)-5-chlorobenzonitrile (0.936 g, 2.079 mmol) as a solution in 20% methanol in chloroform (300 mL) was added 1N HCl (2.079 mL, 2.079 mmol), and the resulting mixture was then concentrated under reduced pressure. The resulting white paste was diluted with acetonitrile (100 mL) and the solvent evaporated in vacuo. The dilution-evaporation was repeated twice more for a total of three times. The resulting residue was placed under vacuum overnight to give product. 1H NMR (DMSO-d6): 6.7.91 (s, 1H), 7.81 (s, 3H), 7.68-7.60 (m, 2H), 7.48 (s, 1H), 7.37 (s, 1H), 6.50-6.30 (m, 2H), 6.00-5.86 (m, 2H). HRMS (M+1)=450.06
WORKUP
后处理
- concentrationthe resulting mixture was then concentrated under reduced pressure
- additionThe resulting white paste was diluted with acetonitrile (100 mL)
- customthe solvent evaporated in vacuo
- customThe dilution-evaporation
- customwas placed under vacuum overnight
- customto give product