HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-chloro-6-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-2-methylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 1H-1,2,4-Triazole, 3,5-dimethyl- | HCID 139001 | — |
| Reactant | 4,6-Dichloro-2-methylpyrimidine | HCID 234997 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-chloro-6-(3,5-dimethyl-1H-1,2,4-triazol-1-yl)-2-methylpyrimidine | HCID 62481745 | 69% |
Reaction Steps
4,6-dichloro-2-methylpyrimidine (2-1) (137.8 g, 845 mmol), 3,5-dimethyl-1H-1,2,4-triazole (2-2) (82 g, 845 mmol), and Cs2CO3 (275 g, 845 mmol) were suspended in DMF (1 L) and the resulting mixture was stirred at room temperature for 66 h. The mixture was then poured into water (2 L) and stirred for 1 hour. The precipitate was filtered, washed with water (2×) and dried under vacuum to afford Intermediate 2 as an off-white solid (130 g, 69%). MS: m/z=224.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09365562B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-1f8731c7f7a842739298a980d3b853d3 |
| Source note | uspto-grants-2016_06 |