HRID750128
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 6-chloro-2-methylamino-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (800 mg), potassium carbonate (400 mg), methyl iodide (20 ml) and DMF (20 ml) was stirred at 80° C. for 3 days. The reaction mixture was concentrated, and ethyl acetate was added to the obtained residue. The mixture was washed with water and brine, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1) and crystallized from isopropyl ether to give the title compound (469 mg) as colorless crystals.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- additionethyl acetate was added to the obtained residue
- washThe mixture was washed with water and brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1)
- customcrystallized from isopropyl ether