反应详情

温度

150 °C

4-(2,6-Difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid (2-amino-3-hydroxymethyl-phenyl)-amide (100 mg, 0.26 mmol) was dissolved in acetic acid (10 ml) then heated for 10 min at 150° C. (100 W) in a CEM discover microwave synthesiser. The reaction mixture was reduced then azeotroped with toluene (2×20 ml). The residue was purified by flash column chromatography [SiO2, EtOAc-hexane (1:1, 2:1, 3:1)] to give 2,6-difluoro-N-[3-(4-hydroxymethyl-1H-benzimidazol-2-yl)-1H-pyrazol-4-yl]-benzamide (25 mg) as an off white solid (LC/MS: Rt 2.70, [M+H]+ 370) and acetic acid 2-[4-(2,6-difluoro-benzoylamino)-1H-pyrazol-3-yl]-1H-benzimidazol-4-ylmethyl ester (20 mg) as an off white solid. (LC/MS: Rt 3.60, [M+H]+ 412).

1. customThe reaction mixture was reduced then azeotroped with toluene (2×20 ml)
2. customThe residue was purified by flash column chromatography [SiO2, EtOAc-hexane (1:1, 2:1, 3:1)]