HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylamine → 4-Chloro-N-methylpicolinamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylamine | HCID 6329 | — |
| Edukt | 4-Chloropyridine-2-carbonyl chloride--hydrogen chloride (1/1) | HCID 22397270 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 4-Chloro-N-methylpicolinamide | HCID 1476814 | — |
Reaktionsschritte
4-Chloropyridine-2-carbonyl chloride HCl salt (7.0 g, 32.95 mmol) was added in portions to a mixture of a 2.0 M methylamine solution in THF (100 mL) and MeOH (20 mL) at 0° C. The resulting mixture was stored at 3° C. for 4 h, then concentrated under reduced pressure. The resulting nearly dry solids were suspended in EtOAc (100 mL) and filtered. The filtrate was washed with a saturated NaCl solution (2×100 mL), dried (Na2SO4) and concentrated under reduced pressure to provide 4-chloro-N-methyl-2-pyridinecarboxamide as a yellow, crystalline solid (4.95 g, 88%): mp 37-40° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08841330B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-e436117fe9344484a9d22d3fbe3def21 |
| Quellennotiz | uspto-grants-2014_09 |