HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acrylamide → 3-(4-(4-(5-Chloro-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidin-2-ylamino)-2,5-dimethylphenyl)piperidin-1-yl)propanamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acrylamide | HCID 6579 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-chloro-N-(2,5-dimethyl-4-(piperidin-4-yl)phenyl)-N4-(5-methyl-1H-pyrazol-3-yl)pyrimidine-2,4-diamine | HCID 58254900 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 3-(4-(4-(5-Chloro-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidin-2-ylamino)-2,5-dimethylphenyl)piperidin-1-yl)propanamide | HCID 58254905 | — |
Reaction Steps
A solution of 5-chloro-N2-(2,5-dimethyl-4-(piperidin-4-yl)phenyl)-N4-(5-methyl-1H-pyrazol-3-yl)pyrimidine-2,4-diamine (41 mg, 0.1 mmol), acrylamide (24 mg, 0.33 mmol) and DIEA (87 μL, 0.5 mmol) in NMP (1 mL) was stirred at 80° C. for 10 h. LCMS at this point shows the reaction was not complete, so additional acrylamide (2×36 mg) was added and the reaction continued until LCMS shows the reaction was complete. The crude product was purified by RP-HPLC to give 3-(4-(4-(5-Chloro-4-(5-methyl-1H-pyrazol-3-ylamino)pyrimidin-2-ylamino)-2,5-dimethylphenyl)piperidin-1-yl)propanamide as a white powder; ESMS m/z 483.2 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08519129B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-ab9d48f0a6f84b188ac88d0cddbf6c5f |
| Source note | uspto-grants-2013_08 |