HRID2060855
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
- 70 °C
PROCEDURE
实验过程
To a solution of 1-chloro-4-hydroxyisoquinoline (1.0 g, 5.6 mmol) in DMF (16 mL), was added 6-chloronicotinonitrile (0.55 g, 4.0 mmol) and K2CO3 (1.65 g, 11.9 mmol). The reaction mixture was heated at 70° C. for 6.5 h. Solvent was removed in vacuo and residue partitioned between EtOAc (100 mL), THF (100 mL) and water (60 mL). The organic phase was washed with water (2×60 mL), 1M NaOH (2×40 mL), brine (40 mL) and dried (MgSO4). Solvent was removed in vacuo to give the title compound: RT=3.66 min; m/z (ES+)=282.0 [M+H]+.
WORKUP
后处理
- customSolvent was removed in vacuo and residue
- custompartitioned between EtOAc (100 mL), THF (100 mL) and water (60 mL)
- washThe organic phase was washed with water (2×60 mL), 1M NaOH (2×40 mL), brine (40 mL)
- dry with materialdried (MgSO4)
- customSolvent was removed in vacuo