HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylamine → 2-chloro-N-methyl-5-nitropyrimidin-4-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylamine | HCID 6329 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 2,4-Dichloro-5-nitropyrimidine | HCID 521266 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-chloro-N-methyl-5-nitropyrimidin-4-amine | HCID 7147232 | 100% |
Reaktionsschritte
To a solution of 2,4-dichloro-5-nitropyrimidine (5 g, 26 mmol) in THF (50 mL) was added diisopropylethylamine (3.36 g, 26 mmol) at −78° C., followed by the dropwise addition of methylamine (13 mL, 2 mol/L in methanol, 26 mmol). After the addition, the mixture was warmed to RT and stirred for 3 h. The reaction mixture was then diluted with ethyl acetate and washed with brine (50 mL*3). The organic layer was dried over sodium sulfate, filtered and concentrated to give the title compound (4.4 g, 100%) as a yellow solid. MS (ES+) C5H5ClN4O2 requires: 188, 190. found: 189, 191 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09340514B2 |
| Quelldatensatz | uspto-grants-2016_05 |
| ORD ID | ord-0743059575294e81abd40c482cef0bd1 |
| Quellennotiz | uspto-grants-2016_05 |