Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | HCID 89442706 | HCID 89442706 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 89442639 | HCID 89442639 | — |
Reaction Steps
To a solution of 4-amino-6-{4-[1-azetidin-3-ylmethyl-4-(4-fluoro-3-trifluoromethyl-phenyl)-1H-imidazol-2-yl]-piperidin-1-yl}-pyrimidine-5-carboxylic acid amide trifluoroacetate (2) (25.00 mg; 0.03 mmol; 1.00 eq.) in ethanol 1 ml added formic acid (0.00 1 ml; 0.08 mmol; 2.50 eq.) and formaldehyde (0.001 ml; 0.04 mmol; 1.20 eq.), stirred at 65° C. for 3 hr. lc-ms showed clean desired peak. Removed off solvent, purified by HPLC, collected title compound 14.8 mg. LC-MS (M+1=533, obsd.=533).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09145392B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-01c27987fa5a4f908bdc77f979fd8586 |
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| Source note | uspto-grants-2015_09 |
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