HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-Methylbutylamine → 4-[[(N-methyl-N-butylamino)methylene]amino]-3-pyridinol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-Methylbutylamine | HCID 8068 | — |
| Edukt | Ammonium Sulfate | HCID 6097028 | — |
| Edukt | 4-[[(Dimethylamino)methylene]amino]-3-pyridinol | HCID 15380929 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 4-[[(N-methyl-N-butylamino)methylene]amino]-3-pyridinol | HCID 15380936 | 64,2% |
Reaktionsschritte
A mixture of 4-[[(dimethylamino)methylene]amino]-3-pyridinol (7.50 g), N-methylbutylamine (8.10 g), ammonium sulfate (0.600 g), and anhydrous toluene (25 mL) was heated at reflux under nitrogen for 2.25 hours. The solution was concentrated under reduced pressure and the crude product chromatographed on silica gel (10% methanol in dichloromethane) to afford 6.04 g of solid. Recrystallization from ethyl acetate/hexanes afforded 3.90 g of a crystalline material, m.p. 83°-85° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05866565 |
| Quelldatensatz | uspto-grants-1999_02 |
| ORD ID | ord-6e22c930eead4c0796553d715110e389 |
| Quellennotiz | uspto-grants-1999_02 |