Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | E-1210 | HCID 16719049 | — |
| Solvent | tert-Butyl methyl ether | HCID 15413 | — |
| Product | HCID 25070440 | HCID 25070440 | 87.2% |
Reaction Steps
To 3-(3-(4-(pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-yl amine (1 g) and citric acid (564 mg) was added methanol (3 mL), and the suspension was stirred at 30 to 35° C, to turn it into a solution. Under stirring at 30° C, after adding tert-butyl methyl ether (3 mL) dropwise over 15 minutes to this solution and seeding, crystals precipitated. After stirring at 30° C for 10 minutes, tert-butyl methyl ether (15 mL) was added at the same temperature for one hour, and after slow cooling, mixture was stirred at 23° C for two hours. The precipitated crystals were filtered and dried to obtain the title compound (1.34 g) as a white crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08058444B2 |
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| Source dataset | uspto-grants-2011_11 |
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| ORD ID | ord-6016b34a1d3f420987ce5153f8c27450 |
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| Source note | uspto-grants-2011_11 |
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