反应详情

509 mg (1,0 mmol) [3-(6,8-Dichloro-2-methyl-1,2,3,4-tetrahydro-isoquinolin-4-yl)-phenyl]-carbamic-acid 4-nitro-phenyl-ester-Hydrochloride (example 151, intermediate 1) were dissolved in 15 ml DMF and at 0° C. a solution of 67,2 mg (1,1 mmol) of 2-Aminoethanol in 10 ml DMF was added. After stirring for 3 h at room temperature the solvent was removed i. vac. The residue was dissolved in ethylacetate and washed with sat. NaHCO3-solution. The organic layer was separated and the aqueous layer was extracted twice with ethylacetate. The combined organic layers were washed with sat. NaCl-solution, dried (MgSO4) and concentrated. Purification by silica gel chromatography (dichloromethane/methanol) yielded 265 mg of the title compound.

1. additionwas added
2. customwas removed i
3. dissolutionThe residue was dissolved in ethylacetate
4. washwashed with sat. NaHCO3-solution
5. customThe organic layer was separated
6. extractionthe aqueous layer was extracted twice with ethylacetate
7. washThe combined organic layers were washed with sat. NaCl-solution
8. dry with materialdried (MgSO4)
9. concentrationconcentrated
10. customPurification by silica gel chromatography (dichloromethane/methanol)