HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylcarbamoyl Chloride → 4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | N,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamide | HCID 15380930 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | 4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamate | HCID 67749077 | 70,3% |
Reaktionsschritte
To a solution prepared from 4-[[(diethylamino)methylene]amino]-3-pyridinol (3.12 g), triethylamine (3.34 g) and tetrahydrofuran (50 mL) was added N,N-dimethylcarbamyl chloride (2.28 g) under nitrogen. The resulting mixture was stirred at ambient temperature for 6 hours, diluted with ether (50 mL) and filtered. The filtrate was concentrated under reduced pressure and the residue chromatographed on silica gel (elution with 10% methanol in dichloromethane) to give 3.00 g of solid. Recrystallization from ether/hexanes afforded 1.57 g of crystalline solid, m.p. 73°-74° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05869480 |
| Quelldatensatz | uspto-grants-1999_02 |
| ORD ID | ord-5329b47efe444ae4a43539aa7a09e764 |
| Quellennotiz | uspto-grants-1999_02 |