Hydrochloric Acid → Methyl 3-fluoromethylpyrazine-2-carboxylate

Temperatur

140 °C

Methyl 3-chloromethylpyrazine-2-carboxylate (1.55 g, 8.3 mmol) was dissolved in DMSO (30 ml), followed by adding cesium fluoride (2.52 g, 16.6 mmol) and hexamethyl triamidophosphate (0.3 ml) and heated at 140° C. for 40 minutes while stirring. The reaction solution was cooled, followed by pouring into a diluted HCl solution, extracting with ethyl acetate, and washing with water. The solution was dried over magnesium sulfate, and concentrated under reduced pressure, and then the residue was purified by using silica gel chromatography (hexane:ethyl acetate=2:1) to obtain 0.13 g of the desired compound.

1. temperatureThe reaction solution was cooled
2. extractionextracting with ethyl acetate
3. washwashing with water
4. dry with materialThe solution was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customthe residue was purified

ORD-Eintrag

ord-6ee773351ce04e88bb96aa9523a258b1

Quelldatensatz

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08269045B2