Fluorine → Methyl 3-chloro-6-fluoropyrazine-2-carboxylate

In 15 mL of acetonitrile was dissolved 0.3 g of methyl 3-chloro-2-pyrazinecarboxylate. At an ice-cooled temperature, 10% fluorine gas (a fluorine gas diluted with nitrogen gas) was introduced at a rate of 45 ml per minute for a period of 18 minutes. Then, while elevating the temperature from the ice-cooled temperature to room temperature, nitrogen gas was introduced for one hour, and the reaction product was concentrated under reduced pressure. The oily product thus obtained was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=10:1] to obtain 0.03 g of methyl 3-chloro-6-fluoro-2-pyrazinecarboxylate as a colorless oily product.

1. additiondiluted with nitrogen gas)
2. additionwas introduced at a rate of 45 ml per minute for a period of 18 minutes
3. additionnitrogen gas was introduced for one hour
4. concentrationthe reaction product was concentrated under reduced pressure
5. customThe oily product thus obtained
6. customwas purified by silica gel column chromatography (eluent

ORD record

ord-4924200c578f4305a9f554ebf31323c7

Source dataset

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06800629B2