HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 69036476, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | HCID 69039109 | HCID 69039109 | — |
| Product | HCID 69036476 | HCID 69036476 | 23% |
Reaction Steps
Using a procedure analogous to example A1, 1-(3-tert-butyl-1-methyl-1H-pyrazol-5-yl)-3-(4-chloro-2-fluoro-5-(8-methyl-2-(methylthio)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-6-yl)phenyl)urea (0.2, 0.38 mmol) and 2 M methylamine in THF (3 eq) were combined and purified via C-18 chromatography to provide 1-(3-tert-butyl-1-methyl-1H-pyrazol-5-yl)-3(4-chloro-2-fluoro-5-(8-methyl-2-(methylamino)-7-oxo-7,8-dihydropyrido[2,3-d]pyrimidin-6-yl)phenyl)urea as a white solid (0.045 g, 23% yield). 1H NMR (400 MHz, DMSO-d6): δ 8.95 (brs, 2H), 8.61 (s, 1H), 8.17 (d, J=8.8 Hz, 1H), 7.87 (brs, 1H), 7.75 (s, 1H), 7.55 (d, J=10.8 Hz, 1H), 6.04 (s, 1H), 3.58-3.51 (m, 6H), 2.90 (s, 3H), 1.16 (s, 9H); MS (ESI) m/z: 513.3 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08188113B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-23b5203c88c545bfb36c5cefde52d79e |
| Source note | uspto-grants-2012_05 |