HRID2060858
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
- 80 °C
PROCEDURE
实验过程
To 6-(1-methylisoquinolin-4-yloxy)nicotinamide (Preparation 19) (135 mg, 0.48 mmol) in dioxane (6 mL) under argon was added selenium dioxide (54 mg, 0.48 mmol). The mixture was heated to 80° C. for 3 h after which time selenium dioxide (54 mg, 0.48 mmol) was added. After a further 0.5 h at 80° C. the mixture was cooled, filtered through Celite and washed with EtOAc (50 mL). The organic phase was washed with NaHCO3 (30 mL), water (30 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo to give the title compound: RT=2.93 min; m/z (ES+)=294.1 [M+H]+.
WORKUP
后处理
- additionwas added
- filtrationfiltered through Celite
- washwashed with EtOAc (50 mL)
- washThe organic phase was washed with NaHCO3 (30 mL), water (30 mL), brine (30 mL)
- dry with materialdried (MgSO4)
- customSolvent was removed in vacuo