Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Propylamine | HCID 7852 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | L-Proline | HCID 145742 | — |
| Reactant | HCID 67202884 | HCID 67202884 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 59856859 | HCID 59856859 | 37% |
Reaction Steps
4-[5-Cyano-6-(2-fluoro-4-iodo-phenylamino)-pyrimidin-4-yloxy]-piperidine-1-carboxylic acid isopropyl ester (250 mg, 0.48 mmol), n-propylamine (408 μL, 4.8 mmol), proline (99 mg, 0.86 mmol), copper iodide (92 mg, 0.48 mmol) and potassium carbonate (152 mg, 1.1 mmol) were mixed together in DMSO (4 mL). The reaction vessel was heated in a microwave at 80° C. for 30 minutes. Progress of the reaction was monitored by TLC and LCMS. Purification by HPLC afforded compound A64 as a white solid (80 mg, 37%). 1H NMR (CDCl3, 400 MHz) δ 9.37 (s, 1H), 8.22 (s, 1H), 6.91 (t, 1H), 6.91 (m, 2H), 5.27 (h, 1H), 4.71 (h, 1H), 3.53 (m, 2H), 3.23 (m, 2H), 2.91 (m, 2H), 1.85 (m, 2H), 1.54 (m, 4H), 1.13 (d, 6H), 0.88 (t, 3H). Exact mass calculated for C23H29FN6O3 456.51, found 457.4 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07470699B2 |
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| Source dataset | uspto-grants-2008_12 |
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| ORD ID | ord-74e032dec88047f7ba11072f42b43f5c |
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| Source note | uspto-grants-2008_12 |
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