HRID1095294
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of the product from Step 2 (7-bromo-6-methoxyisoquinolin-1(2H)-one) (4.7 g, 18.5 mmol) in phosphorus oxychloride (30 mL) was heated to reflux for 2 hours and cooled to RT. The volatiles were then evaporated, and the residue was partitioned between 3 M NaOH and DCM. The organic phase was dried over Na2SO4; the solvent was evaporated; and the solid was triturated with Et2O (20 mL) and filtered to give a solid (3.75 g). LRMS ESI+ (M+H)+274.0.
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux for 2 hours
- customThe volatiles were then evaporated
- customthe residue was partitioned between 3 M NaOH and DCM
- dry with materialThe organic phase was dried over Na2SO4
- customthe solvent was evaporated
- customand the solid was triturated with Et2O (20 mL)
- filtrationfiltered