反应详情

温度

140 °C

To a solution of N-(2-amino-2-methylcyclopentyl)-2-(2H-1,2,3-triazol-2-yl)benzamide hydrochloride (Intermediate 26; 287 mg, 1.01 mmol) in dry DMSO (3.4 ml) was added 2-chloro-5-(trifluoromethyl)pyrazine (CAS number 799557-87-2; 202 mg, 1.11 mmol) and DIPEA (527 μl, 3.02 mmol). The reaction was stirred at 140° C. for 1 hour and was then partitioned between ethyl acetate and water. The organics were washed with water, brine, filtered through a hydrophobic frit and concentrated in vacuo. This was purified by column chromatography (silica, 0-100% ethyl acetate/petrol then 0-20% methanol/ethyl acetate) and was then recrystallised from ethyl acetate to afford the title compound.

1. customwas then partitioned between ethyl acetate and water
2. washThe organics were washed with water, brine
3. filtrationfiltered through a hydrophobic frit
4. concentrationconcentrated in vacuo
5. customThis was purified by column chromatography (silica, 0-100% ethyl acetate/petrol
6. custom0-20% methanol/ethyl acetate) and was then recrystallised from ethyl acetate