Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86712908 | HCID 86712908 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86712909 | HCID 86712909 | 111.9% |
Reaction Steps
A solution of the compound (315 mg, 0.59 mmol) obtained in Example 43-1) 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 (279 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-48af1f6b76a44c4f929bd3ea07c3cf5a |
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| Source note | uspto-grants-2015_01 |
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