HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,6-Dichloropyrimidine → 6-Chloro-N-(4-methoxybenzyl)pyrimidin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | 4-Methoxybenzylamine | HCID 75452 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | 6-Chloro-N-(4-methoxybenzyl)pyrimidin-4-amine | HCID 22309497 | 91.5% |
Reaction Steps
A mixture of 4,6-dichloropyrimidine (Aldrich, 3.6 g, 24.2 mmol), 4-methoxybenzylamine (2.7 g, 19.7 mmol), DIPEA (5 ml, 28.8 mmol), and n-BuOH was heated at reflux for 3 h. The mixture was concentrated and the residue treated with H2O (150 mL) and EtOAc (175 mL). The EtOAc phase was separated, washed with saturated aq. NaHCO3 solution and brine, dried (MgSO4), and concentrated to give the title compound (4.5 g) which was used without further purification. 1H NMR (DMSO-d6) δ 8.29 (s, 1H), 8.13 (br s, 1H), 7.25 (d, 2H, J=8.2 Hz), 6.90 (d, 2H, J=8.2 Hz), 6.56 (s, 1H), 4.48 (s, 2H), 3.75 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07459562B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-00c5073b629944198f8b25052d84e059 |
| Source note | uspto-grants-2008_12 |