Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 44137083 | HCID 44137083 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68771419 | HCID 68771419 | — |
Reaction Steps
50 mg of tert-butyl(3S)-3-{4-[7-(aminocarbonyl)-2H-indazol-2-yl]phenyl}piperidine-1-carboxylate (Example 1, D3) as a compound stock solution was reacted with 1 mole equivalent of fumaric acid, added as a 0.405 Molar solution in ethanol. Excess solvent was removed under centrifugal evaporation and 1 mL of ethanol added at ambient room temperature (˜25° C.). The resultant solution stirred at 40° C. for 24 hours. The experiment was left to gently evaporate under atmospheric conditions where a colorless solid was observed. This solid was analyzed using x-ray powder diffraction, proton NMR, DSC and TGA to confirm the formation of the title salt.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08436185B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-6a35c0bfec054d4398451050c4b957fa |
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| Source note | uspto-grants-2013_05 |
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