反应详情

A mixture of 5-methyl-3-phenylisoxazole-4-carboxylic acid (57 mg, 0.28 mmol), 3-(1H-benzimidazol-2-yl)-1H-pyrazol-4-ylamine (50 mg, 0.25 mmol), EDC (58 mg, 0.30 mmol) and HOBt (41 mg, 0.30 mmol) in DMSO (2 ml) was stirred at ambient temperature for 24 h. The reaction mixture was partitioned between EtOAc and water and the organic portion dried (MgSO4), filtered and reduced in vacuo. The residue was purified by flash column chromatography [SiO2, EtOAc-petrol (1:2, 1:1, 2:1)] affording 5-methyl-3-phenyl-isoxazole-4-carboxylic acid [3-(1H-benzimidazol-2-yl)-1H-pyrazol-4-yl]-amide as a cream solid (15 mg, 16%). (LC/MS: Rt 3.73, [M+H]+ 385.14).

1. customThe reaction mixture was partitioned between EtOAc and water
2. dry with materialthe organic portion dried (MgSO4)
3. filtrationfiltered
4. customThe residue was purified by flash column chromatography [SiO2, EtOAc-petrol (1:2, 1:1, 2:1)]