反应详情

温度

140 °C

Methyl 2-(4′-(6-carbamoyl-3,5-dimethylpyrazin-2-yl)-2-chlorobiphenyl-4-yl)acetate (Intermediate 1-1; 60 mg, 0.15 mmol) and ammonia (7M in methanol) (2091 μL, 14.64 mmol) were sealed into a microwave tube. The reaction was heated to 140° C. for 1 hour in the microwave reactor and cooled to RT. Removal of the solvent under reduced pressure gave crude product. The crude product was purified by preparative HPLC (Waters—Xbridge Prep C18 5 μm), using decreasingly polar mixtures of water (containing 0.1% formic acid) and {MeOH(3):MeCN(1)} as eluents. Fractions containing the desired compound were evaporated to dryness to afford 6-(4′-(2-amino-2-oxoethyl)-2′-chlorobiphenyl-4-yl)-3,5-dimethylpyrazine-2-carboxamide (16.20 mg, 28.0%) as a colourless solid.

1. temperaturecooled to RT
2. customRemoval of the solvent under reduced pressure
3. customgave crude product
4. customThe crude product was purified by preparative HPLC (Waters—Xbridge Prep C18 5 μm)
5. additionFractions containing the desired compound
6. customwere evaporated to dryness