HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-N-(3-bromophenyl)-7-N-methylpyrido[2,3-d]pyrimidine-4,7-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-(3-bromophenyl)-7-fluoropyrido[2,3-d]pyrimidin-4-amine | HCID 5328268 | — |
| Reactant | Methylamine hydrochloride | HCID 6364545 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-N-(3-bromophenyl)-7-N-methylpyrido[2,3-d]pyrimidine-4,7-diamine | HCID 5328269 | 77% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A solution of 4-(3-bromoanilino)-7-fluoropyrido[2,3-d]pyrimidine (see a previous experimental) (0.20 g, 0.63 mmol), methylamine hydrochloride (0.13 g, 1.88 mmol) and Et3N (0.30 mL) 2.19 mmol) in EtOH (15 mL) is heated at 100° C. in a pressure vessel for 18 h. The solvent is removed under reduced pressure, and the residue is partitioned between EtOAc and water. Workup of the organic layer gives 4-(3-bromoanilino)-7-(methylamino)pyrido[2,3-d]pyrimidine (0.16 g, 77%). 1H NMR (DMSO) δ 9.53 (1H, s), 8.54 (1H, s), 8.41 (1H, d, J=8.1 Hz), 8.17 (1H, t, J=1.8 Hz), 7.83 (1H, dd, J=8.0, 1.9 Hz), 7.66 (1H, brs), 7.32 (1H, t, J=8.0 Hz), 7.24 (1H, dd, J=8.0, 1.8 Hz), 6.77 (1H, d, J=8.1 Hz), 2.92 (3H, d, J=4.8 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654307 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-92f343ca243b4c739767a9abc36a3623 |
| Source note | uspto-grants-1997_08 |