HRID1609593
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 84 ml of 47% aqueous hydrogen bromide was added 11.3 g of 3,4-dihydro-7-methoxy-2-(3-pyridylmethyl)-1 (2H)-isoquinolinone, and the mixture was refluxed under heating for 4.5 hours. After ice cooling, the mixture was neutralized with aqueous sodium hydroxide, made weakly acidic with acetic acid and shaken with ethyl acetate. The organic layer was washed with water and saturated brine in order, dried over anhydrous magnesium sulfate and concentrated in vacuo. The resultant residue was chromatographed on a column of silica gel, eluting with ethyl acetate to give 5.00 g of the titled compound.
WORKUP
后处理
- temperaturethe mixture was refluxed
- temperatureunder heating for 4.5 hours
- washThe organic layer was washed with water and saturated brine in order
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
- customThe resultant residue was chromatographed on a column of silica gel
- washeluting with ethyl acetate