HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-(4-Methylpiperazin-1-yl)aniline → 6-Bromo-8-ethyl-2-[[4-(4-methylpiperazin-1-yl)phenyl]amino]-8H-pyrido[2,3-d]pyrimidin-7-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-(4-Methylpiperazin-1-yl)aniline | HCID 737253 | — |
| Reactant | 6-Bromo-8-ethyl-2-methylsulfinylpyrido[2,3-d]pyrimidin-7-one | HCID 67119610 | — |
| Product | 6-Bromo-8-ethyl-2-[[4-(4-methylpiperazin-1-yl)phenyl]amino]-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 66760454 | 40.5% |
Reaction Steps
6-Bromo-8-ethyl-2-methanesulfinyl-8H-pyrido[2,3-d]pyrimidin-7-one (4, 600 mg, 1.90 mmol) and 4-(4-methylpiperazino)aniline (363 mg, 1.90 mmol) were stirred at 120° C. for 3 h. The reaction mixture was purified by column chromatography using dichloromethane:methanol (100:3→100:5) to give the title compound (340 mg, 0.77 mmol, 40%) as a yellow solid. ESMS m/z 443 (M+H)+; 1H NMR (400 MHz, CDCl3) δ ppm 8.47 (s, 1H) 7.92 (s, 1H) 7.51 (d, J=8.8 Hz, 2H) 7.24 (br. s., 1H) 6.96 (d, J=8.8 Hz, 2H) 4.48 (q, J=7.0 Hz, 2H) 3.13-3.29 (m, 4H) 2.53-2.64 (m, 4H) 2.36 (s, 3H) 1.35 (t, J=7.0 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08372970B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-3d3ee01b5907479daa49ccd078d90bcf |
| Source note | uspto-grants-2013_02 |