Calcium Carbonate → HCID 178513810, compound

In 200 mL of water was suspended 1.0 g of 3-hydroxy-2-pyrazinecarboxamide. At room 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 25 minutes. Then, nitrogen gas was introduced for 45 minutes, and the liquid reaction mixture was neutralized with calcium carbonate, the deposited precipitate was filtered off, the filtrate was concentrated under reduced pressure, and the solid product thus obtained was purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1] to obtain 0.008 g of 6-fluoro-3-hydroxy-2-pyrazinecarboxamide as a white-colored solid product.

1. additionwas introduced at a rate of 45 mL per minute for a period of 25 minutes
2. additionThen, nitrogen gas was introduced for 45 minutes
3. customthe liquid reaction mixture
4. filtrationthe deposited precipitate was filtered off
5. concentrationthe filtrate was concentrated under reduced pressure
6. customthe solid product thus obtained
7. customwas purified by silica gel column chromatography [eluent: n-hexane:ethyl acetate=5:1]

ORD record

ord-db244f86290d46ee90463e77e2bc6cfb

Source dataset

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06800629B2