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HRID 399396Erstellt: 24. Oktober 2026

Dimethylcarbamoyl Chloride → 4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamate

https://huagongshe.com/de/reaction/399396

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktDimethylcarbamoyl ChlorideHCID 6598—
EduktTetrahydrofuranHCID 8028—
EduktTriethylamineHCID 8471—
EduktN,N-Diethyl-N'-(3-hydroxypyridin-4-yl)methanimidamideHCID 15380930—
LösungsmittelDiethyl EtherHCID 3283—
Produkt4-[[(Diethylamino)methylene]amino]-3-pyridinol N,N-dimethyl carbamateHCID 6774907770,3%

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

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS05821239
Quelldatensatzuspto-grants-1998_10
ORD IDord-d499d14d330d400ba93eabe225f7d895
Quellennotizuspto-grants-1998_10