Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86712898 | HCID 86712898 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86712899 | HCID 86712899 | 104% |
Reaction Steps
A solution of the compound (217 mg, 0.43 mmol) obtained in Example 38-1) and 4 M hydrochloric acid (1,4-dioxane solution, 1 mL) in methanol (4 mL) was stirred at room temperature for 16 h. The reaction mixture was concentrated under reduced pressure, saturated aqueous sodium hydrogencarbonate was added to the residue, the mixture was extracted with dichloromethane, and the organic layer was washed with saturated sodium chloride solution and dried with anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel chromatography (Isco Combiflash, 12 g, methanol:ethyl acetate=0:100 to 40:60, gradient) to obtain the title compound (176 mg, quant.) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08927536B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-5b31a487d6604c359871a4f3ba97f11d |
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| Source note | uspto-grants-2015_01 |
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