Fluorine → HCID 22662772, compound

In 15 mL of acetonitrile was dissolved 0.3 g of 3-chloro-2-pyrazinecarbonitrile. At an ice-cooled temperature, 10% fluorine gas (a fluorine gas diluted with nitrogen gas) was introduced into the solution at a rate of 45 mL per minute for a period of 20 minutes. Then, while elevating the temperature from the ice-cooled temperature to room temperature, nitrogen gas was introduced over a period of one hour. The reaction mixture was concentrated under reduced pressure and the oily product thus obtained was purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=10:1] to obtain 0.12 g of 3-chloro-6-fluoro-2-pyrazinecarbonitrile as a colorless oily product.

1. additiondiluted with nitrogen gas)
2. additionwas introduced into the solution at a rate of 45 mL per minute for a period of 20 minutes
3. additionnitrogen gas was introduced over a period of one hour
4. concentrationThe reaction mixture was concentrated under reduced pressure
5. customthe oily product thus obtained
6. customwas purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=10:1]

ORD record

ord-1b15075871764691b6cea4baea93de6f

Source dataset

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06800629B2