HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 4-N-(3-bromophenyl)-7-N,7-N-dimethylpyrido[4,3-d]pyrimidine-4,7-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | N-(3-bromophenyl)-7-fluoropyrido[4,3-d]pyrimidin-4-amine | HCID 5328251 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 4-N-(3-bromophenyl)-7-N,7-N-dimethylpyrido[4,3-d]pyrimidine-4,7-diamine | HCID 5328253 | 94% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of 7-fluoro-4-(3-bromoanilino)pyrido[4,3-d]pyrimidine (101 mg, 0.32 mmol), triethylamine (4.4 mL, 32 mmole) and dimethylamine hydrochloride (2.58 g, 32 mmol) in isopropanol (30 mL) contained in a steel bomb is stirred at 100° C. (oil bath) for 4 h. The resulting solution is concentrated under vacuum, basified with aqueous Na2CO3 and diluted with water to give a solid. Filtration and recrystallisation from MeOH/CHCl3 gives 7-dimethylamino-4-(3-bromoanilino)pyrido[4,3-d]pyrimidine (102 mg, 94%) as a pale yellow solid. 1H NMR (DMSO) δ 9.93 (1H, brs), 9.42 (1H, s), 8.48 (1H, s), 8.19 (1H, s), 7.85 (1H, d, J=7.7 Hz), 7.35 (1H, t, J=7.9 Hz), 7.30 (1H, brd, J=7.8 Hz), 6.53 (1H, s), 3.16 (6H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654307 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-cdc4e33b2294490c91182c3c3cabe2a1 |
| Source note | uspto-grants-1997_08 |