Methanesulfonate → HCID 66965377, compound

To a solution of the compound prepared in Example 3 (537 mg) in ethanol (4 mL) was added tin chloride dihydrate (2.07 g) and the mixture was refluxed for 30 minutes. After cooling to room temperature, a saturated aqueous sodium hydrogen carbonate solution was added to the reaction mixture, which was extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated. To methanol (2 mL) was added the obtained solid (137 mg) and then 4N hydrogen chloride in dioxane (0.26 mL) was added to the mixture, which was stirred at room temperature for 3 hours. The reaction mixture was concentrated. The residue was recrystallized from a mixture solvent (isopropanol:ethanol=4:1) to give the compound of the present invention (144 mg) having the following physical data. Moreover, the compound was converted to methanesulfonate thereof by conventional method.

1. temperaturethe mixture was refluxed for 30 minutes
2. extractionwas extracted with ethyl acetate
3. washThe extract was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated
6. additionTo methanol (2 mL) was added the obtained solid (137 mg)
7. addition4N hydrogen chloride in dioxane (0.26 mL) was added to the mixture, which
8. concentrationThe reaction mixture was concentrated
9. customThe residue was recrystallized from a mixture solvent (isopropanol:ethanol=4:1)
10. customto give the compound of the present invention (144 mg)

ORD record

ord-f3490aa322ba407a929bbcc27475358e

Source dataset

uspto-grants-2008_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07402580B2