Reaktion #2139332

Reaktionsgleichung

formic acid

furamide

phosphorus pentachloride

HCl

→

N-[Dichlorophosphinyl]-2-furamide

Lösungsmittel

carbon tetrachloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturCooled to 30°
2. 2
   Filtrationbefore filtering
3. 3
   WaschenThe product was washed with AR carbon tetrachloride
4. 4
   Sonstigeair-dried
5. 5
   Sonstigeto give 17.8 g
6. 6
   Sonstigem.p. softens 83°
7. 7
   Sonstigemelts 93°-112°

Vorschrift

A mixture of 11.1 g (0.1 mole) of furamide, 20.8 g (0.1 mole) of phosphorus pentachloride and 150 ml of AR carbon tetrachloride was heated at 70° for 30 min. or until the HCl gas evolution had ceased. Cooled to 30° and 4.7 g (0.1 mole) of 97% formic acid was added dropwise. Stirring was continued for 45 min., before filtering. The product was washed with AR carbon tetrachloride and air-dried to give 17.8 g, m.p. softens 83°, melts 93°-112°.

Quelle