Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86712921 | HCID 86712921 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86712923 | HCID 86712923 | 79.1% |
Reaction Steps
The compound (348 mg, 0.67 mmol) obtained in Example 52-3) was dissolved in methanol (3 mL). A 4 N solution (1.67 mL) of hydrochloric acid in dioxane was added to the solution, and the mixture was stirred at room temperature for 1 h. The solvent was distilled off, the residue was dissolved in a mixed solvent of methylene chloride (50 mL) and methanol (2 mL), and the mixture was separated into organic and aqueous layers by the addition of saturated aqueous sodium hydrogencarbonate (20 mL). The organic layer was washed with saturated sodium chloride solution and then dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained residue was purified by silica gel column chromatography (elution solvent: methanol/ethyl acetate=10% to 60%) to obtain the title compound (216 mg, 79%) in a white solid form.
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-45aeb06194734641be77c5ef283c4e2b |
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| Source note | uspto-grants-2015_01 |
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