HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 6-Chloro-N4-(3-nitrobenzyl)pyrimidine-2,4,5-triamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,5-Diamino-4,6-dichloropyrimidine | HCID 301039 | — |
| Reactant | Benzenemethanamine, 3-nitro-, hydrochloride (1:1) | HCID 2724030 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | 6-Chloro-N4-(3-nitrobenzyl)pyrimidine-2,4,5-triamine | HCID 86611048 | 78.6% |
Reaction Steps
A mixture of 4,6-dichloropyrimidine-2,5-diamine (700 mg, 3.91 mmol), 3-nitrobenzylamine hydrochloride (885 mg, 4.69 mmol) and triethylamine (1.6 mL, 11.7 mmol) in n-BuOH (20 mL) was refluxed for 17 h, concentrated in vacuo and the residue partitioned between EtOAc (10 mL) and H2O (5 mL). The organic phase was dried (MgSO4) and concentrated in vacuo to give the title compound as an orange solid (906 mg, 76%) which was used in the next reaction without further purification; NMR δH (400 MHz, CDCl3) 8.16 (1H, s), 8.10 (1H, d, J 8.0 Hz), 7.80 (1H, d, J 7.5 Hz), 7.62 (1H, t, J 7.5 Hz), 7.25 (1H, t, J 6.0 Hz), 5.69 (2H, s), 4.67 (2H, d, J 6.0 Hz) and 3.93 (2H, br s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07589097B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-a16a1790f2de4b97990de2675c4e9ad8 |
| Source note | uspto-grants-2009_09 |