反应详情

7-[3-[[(2,3-Dihydro-6-phenylmethoxy-1,4-benzodioxin-2-yl)methyl]amino]propoxy]-2H-1-benzopyran-2-one hydrochloride (0.82 g, 1.6 mmole), prepared in Example 4 above, was dissolved in a mixture of 150 ml of water and 10 ml of methanol, 300 mg of 5% palladium on carbon added, and the mixture hydrogenated at 25 psi on a Parr apparatus for 4.5 hours. It was then filtered through celite and concentrated to dryness in vacuum. The residue was redissolved in methanol and boiled on a hot plate, the methanol being gradually replaced with isopropanol, and an additional 2.8 ml of 4N HCl/isopropanol was added. Upon cooling 0.37 g of the title compound, m.p. 244° C. (d), precipitated as a white solid, monohydrochloride.

1. additionadded
2. filtrationIt was then filtered through celite and
3. concentrationconcentrated to dryness in vacuum
4. dissolutionThe residue was redissolved in methanol
5. additionan additional 2.8 ml of 4N HCl/isopropanol was added
6. temperatureUpon cooling 0.37 g of the title compound, m.p. 244° C. (d)
7. customprecipitated as a white solid, monohydrochloride