HRID1005686
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
- 195 °C
PROCEDURE
实验过程
To 6-ethoxycarbonylamino-1-methyl-3,4-dihydroisoquinoline were added p-cymene (100 ml) and palladium-carbon (0.9 g), followed by heating under stirring at 195° C. in nitrogen atmosphere for 1 hour. After filtering off the catalyst, the reaction mixture was washed with ethanol and a part of the filtrate was evaporated. The residue was extracted with 1N hydrochloric acid, and then basified with potassium carbonate, followed by extracting with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give the title compound (0.629 g, 69%, 2 steps) as pale yellow crystals.
WORKUP
后处理
- temperatureby heating
- filtrationAfter filtering off the catalyst
- washthe reaction mixture was washed with ethanol
- customa part of the filtrate was evaporated
- extractionThe residue was extracted with 1N hydrochloric acid
- extractionby extracting with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was evaporated