反应详情

To a stirred solution of crude (2,2-dimethoxy-ethyl)-[1-[4-(3-hydroxy-propoxy)-3-methoxy-phenyl]-2-(3-methoxy-phenyl)-ethyl]-carbamic acid ethyl ester in acetone (30 mL) was added 6N hydrochloric acid (10 mL) at 0° C. The reaction mixture was stirred at room temperature for 15 hrs. The mixture was diluted with water. The solvent was evaporated and the aqueous layer was extracted with ethyl acetate (3×30 mL). The combined extracts were washed with saturated aqueous sodium chloride solution (20 mL), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 70–230 mesh, 50% ethyl acetate/hexane) afforded 6-(3-hydroxy-propoxy)-7-methoxy-1-(3-methoxy-benzyl)-1H-isoquinoline-2-carboxylic acid ethyl ester (130, 32% yield in two steps) as a colorless oil.

1. customThe solvent was evaporated
2. extractionthe aqueous layer was extracted with ethyl acetate (3×30 mL)
3. washThe combined extracts were washed with saturated aqueous sodium chloride solution (20 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo