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 solution of 3-[({[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)carbonyl]benzoic acid (0.072 g, 0.16 mmol) in DMF (1 mL) was added 1,1-dimethylethyl 4-{[3′-(aminomethyl)-3-biphenylyl]methyl}-1-piperazinecarboxylate (0.061 g, 0.16 mmol), (1-hydroxy-1H-benzotriazolato-O)tri-1-pyrrolidinylphosphorus hexafluorophosphate (0.100 g, 0.192 mmol), and TEA (0.045 mL, 0.320 mmol) and this mixture was stirred at room temperature for 16 h. The resultant mixture was purified using a Gilson HPLC (with 0.1% TFA) and concentrated by GeneVav EZ-2 evaporator to afford the title compound. It was used in the next reaction step without further purification. LC-MS m/z 815 (M+H)+.
WORKUP
后处理
- customThe resultant mixture was purified
- concentrationconcentrated by GeneVav EZ-2 evaporator