Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86712926 | HCID 86712926 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86712927 | HCID 86712927 | 108.9% |
Reaction Steps
A solution of the compound (367 mg, 0.68 mmol) obtained in Example 54-1) 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 20:80, gradient) to obtain the title compound (304 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-f036aad513fd4bf681069be5a0693e6a |
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| Source note | uspto-grants-2015_01 |
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