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
PROCEDURE
实验过程
0.28 g (1 mmol) of 4-acetoxy-8-methoxy-2-methyl-6,7-methylenedioxy-1,2,3,4-tetrahydroisoquinoline (9) was added to 4 ml of ethanol. This solution was then added with 100 mg of 5% palladium carbon and hydrogenated at room temperature. After the reaction was completed, the catalyst was filtered off and the solvent was distilled off under reduced pressure. The residue was added with 5 ml of water and made basic with an aqueous solution of sodium hydroxide. The resulted solution was extracted twice with 5 ml of methylene chloride and the extract was washed with water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 0.19 g of 8-methoxy-2-methyl-6,7-methylenedioxy-1,2,3,4-tetrahydroisoquinoline (13) as a crystal. Yield: 86%.
WORKUP
后处理
- filtrationthe catalyst was filtered off
- distillationthe solvent was distilled off under reduced pressure
- additionThe residue was added with 5 ml of water
- extractionThe resulted solution was extracted twice with 5 ml of methylene chloride
- washthe extract was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure