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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 6-(1-(2,2,2-trifluoroethyl)-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridine (539 mg, 2.02 mmol), tert-butyl 4-(3-bromo-6-iodopyridin-2-yl)-6-hydroxy-1,4-diazepane-1-carboxylate (1.00 g, 2.02 mmol), N1,N2-dimethylethane-1,2-diamine (535 mg, 6.06 mmol), CuI (768 mg, 4.04 mmol), and K2CO3 (1.12 g, 8.08 mmol) in 1,4-dioxane (10 mL) under N2 was heated at 100° C. for 20 hours. The reaction mixture was concentrated under reduced pressure. The residue was purified by silica gel chromatography using EtOAc/petroleum Ether (20%40%) as eluting solvents to afford tert-butyl 4-(3-bromo-6-(6-(1-(2,2,2-trifluoroethyl)-1H-pyrazol-4-yl)-1H-pyrazolo[4,3-c]pyridin-1-yl)pyridin-2-yl)-6-hydroxy-1,4-diazepane-1-carboxylate as a white solid (244 mg, 19%). MS (ESI) m/z: 637 [M+H]+.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure
- customThe residue was purified by silica gel chromatography
- washas eluting solvents