反应详情

1.19 g (5 mmol) of 4-hydroxy-8-methoxy-2-methyl-6,7-methylenedioxy-1,2,3,4-tetrahydroisoquinoline (1) obtained in Reference Example 1 or 2 was dissolved in 15 ml of acetic acid, to which 0.33 ml (6 mmol) of 97% sulfuric acid and 500 mg of 5% palladium on carbon catalyst were added to carry out catalytic reduction at 75° C. for 2 hours. The catalyst was filtered out and 2 ml of 25% aqueous sodium hydroxide solution and 5 ml of water were added to the reaction mixture, which was concentrated under vacuum. 10 ml of water was added to the residue, the solution was made basic with 25% aqueous sodium hydroxide solution and extracted with 10 ml and then 5 ml of methylene chloride successively. The liquid extract was washed with 5 ml of water, dried over anhydrous magnesium sulfate and then concentrated under vacuum to obtain 1.03 g of 8-methoxy-2-methyl-6,7-methylenedioxy-1,2,3,4-tetrahydroisoquinoline. Yield 93%.

1. additionwere added
2. customat 75° C.
3. customfor 2 hours
4. filtrationThe catalyst was filtered out and 2 ml of 25% aqueous sodium hydroxide solution and 5 ml of water
5. additionwere added to the reaction mixture, which
6. concentrationwas concentrated under vacuum
7. addition10 ml of water was added to the residue
8. extractionextracted with 10 ml
9. extractionThe liquid extract
10. washwas washed with 5 ml of water
11. dry with materialdried over anhydrous magnesium sulfate
12. concentrationconcentrated under vacuum