反应详情

温度

50 °C

A solution of 2-(2-pyridyl)-4-methyl-pyrimidine-5-carboxylic acid (559 mg, 2.6 mmol) and 1-amino-5-fluoro-1H-indole-3-carboxylic acid methyl ester (540 mg, 2.6 mmol) in DMF (25 mL) is stirred at 50° C. for 0.5 h. The mixture is treated with DMTMM (718 mg, 2.6 mmol) and stirred at 50° C. for 1 h. The mixture is diluted with saturated aqueous Na2CO3 (50 mL), and extracted with EtOAc (3×50 mL). The combined organic layer is dried (Na2SO4), filtered and concentrated in vacuo. The residue is purified by silica gel chromatography eluting with 1%-10% MeOH in DCM to afford 5-fluoro-1-[(4-methyl-2-pyridin-2-yl-pyrimidine-5-carbonyl)-amino]-1H-indole-3-carboxylic acid methyl ester.

1. extractionextracted with EtOAc (3×50 mL)
2. dry with materialThe combined organic layer is dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue is purified by silica gel chromatography
6. washeluting with 1%-10% MeOH in DCM