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HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 1080858Erstellt: 25. Oktober 2026

Dimethylformamide → N'-(2-Amino-4,6-dichloro-5-pyrimidinyl)-N,N-dimethylmethanimidamide

https://huagongshe.com/reaction/1080858

Reaktionsgleichung

Beteiligte Stoffe

RolleNameHCIDEinwaage
EduktDimethylformamideHCID 6228—
EduktSodium CarbonateHCID 10340—
EduktSodium HydroxideHCID 14798—
EduktPhosphorus oxychlorideHCID 24813—
EduktHCID 178479162HCID 178479162—
LösungsmittelWaterHCID 962—
LösungsmittelTolueneHCID 1140—
ProduktN'-(2-Amino-4,6-dichloro-5-pyrimidinyl)-N,N-dimethylmethanimidamideHCID 1110724995%

Reaktionsbedingungen

Temperatur80 °C

Reaktionsschritte

A suspension of 4.46 g (25 mmol) of diaminodihydroxypyrimidine hydrochloride in 90 ml of toluene and 15.33 g (100 mmol) of phosphorus oxychloride was heated to 80° C. 7.31 g (100 mmol) of dimethylformamide was added drop-wise within a span of 60 minutes. The reaction mixture was then stirred at 80° C. for 16 hours. It was allowed to cool down, and 100 ml of water was then added. The pH was adjusted to 10 using a total of 8.4 g of Na2CO3. The reaction mixture was heated to 40° C. and stirred at this temperature for 4 hours. It was then cooled down to room temperature and neutralized with a 30% solution of NaOH, and the product was filtered off. After washing with water and drying in vacuo, 5.5 g (95%) of product was obtained as a beige solid. This corresponds to a yield of 89%.

Herkunft & Nachweise

DOI10.6084/m9.figshare.5104873.v1
PatentnummerUS05583226
Quelldatensatzuspto-grants-1996_12
ORD IDord-658c42aeb0104a0ab37344691383fad4
Quellennotizuspto-grants-1996_12