反应详情

Under stirring and argon atmosphere [3(6,8-dichloro-2-methyl-1,2,3,4-tetrahydro-isoquinolin-4-yl)-phenyl]-carbamic acid 4-nitro-phenyl ester—hydrochloride salt (15 mg, example 151, intermediate 1) was suspended in dichloromethane (1.5 ml) and 2-dimethylamino-ethanol (3 mg) dissolved in dichloromethane (0.5 ml) was added. After stirring for 6 h and standing over night dichloromethane, water and saturated potassium carbonate solution were added. The organic layer was separated, washed three times with saturated potassium carbonate solution, dried over magnesium sulphate, filtered and concentrated in vacuo. The crude material was purified by preparative HPLC. The product containing fractions were combined and the acetonitrile was removed in vaccuo. After addition of sodium bicarbonate the aqueous phase was extracted with ethyl acetate. The organic layer was separated, dried (magnesium sulphate), filtered and concentrated in vaccuo. The residue was dissolved in water/2N hydrochloric acid and freeze dried to give 5 mg of the title compound.

1. additionwas added
2. stirringAfter stirring for 6 h
3. waitstanding over night
4. customThe organic layer was separated
5. washwashed three times with saturated potassium carbonate solution
6. dry with materialdried over magnesium sulphate
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe crude material was purified by preparative HPLC
10. additionThe product containing fractions
11. customthe acetonitrile was removed in vaccuo
12. additionAfter addition of sodium bicarbonate the aqueous phase
13. extractionwas extracted with ethyl acetate
14. customThe organic layer was separated
15. dry with materialdried (magnesium sulphate)
16. filtrationfiltered
17. concentrationconcentrated in vaccuo
18. dissolutionThe residue was dissolved in water/2N hydrochloric acid
19. customfreeze dried