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ChemicalBook CAS DataBase List 5-Fluoro-isoxazolo[4,5-b]pyrazine-3-carboxylic acid methyl ester
1374986-06-7

5-Fluoro-isoxazolo[4,5-b]pyrazine-3-carboxylic acid methyl ester synthesis

3synthesis methods
5-Fluoro-isoxazolo[4,5-b]pyrazine-3-carboxylic acid methyl ester

1374986-06-7
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Yield:1374986-06-7 44.4%

Reaction Conditions:

with 2,2-difluoro-1,3-dimethyl-imidazolidine in acetonitrile at 80 - 90; for 3 h;Inert atmosphere;

Steps:

6 Synthesis Example 6 Synthesis of (H-1)

Under a nitrogen atmosphere, a mixed solution of 2.00 g (10.3 mmol) of (F-1) and 40.0 mL of acetonitrile was stirred, and 1.88 mL (15.4 mmol) of 2,2-difluoro-1,3-dimethylimidazolidine was then added dropwise thereto. After completion of the dropwise addition, the obtained mixture was stirred at a temperature of 80 to 90° C. for 3 hours. Thereafter, the reaction solution was concentrated under reduced pressure, and the obtained residue was then separated and purified by silica gel chromatography (eluent: hexane/ethyl acetate=2/1 (volume ratio)). As a result, 0.900 g of a white solid (H-1) was obtained. Yield: 44.4%.

References:

US2013/245264,2013,A1 Location in patent:Paragraph 0123