Water → HCID 22247880, compound

Temperature

0 °C

In 4 mL of methanol was dissolved 0.2 g of methyl 3,6-difluoro-2-pyrazinecarboxylate. Then, a 28% methanol solution of sodium methoxide was added at −25° C., and the mixture thus obtained was stirred at 0° C. for 10 minutes. The reaction mixture was poured into a mixture of 30 mL of ethyl acetate and 30 mL of water, and the organic layer was separated. The organic layer thus obtained was washed successively with 15 ml of water and 15 mL of saturated aqueous solution of sodium chloride and dried on anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel chromatography [eluent: n-hexane:ethyl acetate=5:1] to obtain 0.09 g of methyl 6-fluoro-3-methoxy-2-pyrazinecarboxylate as a colorless solid product.

1. customthe mixture thus obtained
2. customthe organic layer was separated
3. customThe organic layer thus obtained
4. washwas washed successively with 15 ml of water and 15 mL of saturated aqueous solution of sodium chloride
5. dry with materialdried on anhydrous magnesium sulfate
6. customthe solvent was removed under reduced pressure
7. customThe residue thus obtained
8. customwas purified by silica gel chromatography [eluent: n-hexane:ethyl acetate=5:1]

ORD record

ord-5cf10171da94486e8b63d5cc3f7f7f61

Source dataset

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06800629B2