Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 2-Pyrrolidone | HCID 12025 | — |
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | (S)-4,6-Dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidin-2-amine | HCID 86659372 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 86659383 | HCID 86659383 | 90.6% |
Reaction Steps
100 mg of (S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine (Reference Example 1), 33 mg of 2-pyrrolidone, 20 mg of 4,5-bis(diphenylphosphino)-9,9′-dimethylxanthene, 149 mg of tripotassium phosphate and 19 mg of tris(dibenzylideneacetone)(chloroform)dipalladium were added in turn to 3 ml of degassed 1,4-dioxane, and the mixture was stirred at 100° C. for 3 hours under argon atmosphere. The reaction solution was filtrated to remove precipitates, and the solvent was distilled off under reduced pressure, and then the obtained residue was purified by silica gel column chromatography to obtain 106 mg of the objective compound as yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08673891B2 |
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| Source dataset | uspto-grants-2014_03 |
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| ORD ID | ord-18b207a0901b4ea6a880f9b3a7acfe10 |
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| Source note | uspto-grants-2014_03 |
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