反应详情

温度

0 °C

2-chloro-6-(4-hydroxypiperidin-1-yl)isonicotinamide (Intermediate 62; 123 mg, 0.48 mmol), 4-bromo-5-methyl-1H-pyrrole-2-carboxylic acid (Intermediate 18) (98 mg, 0.48 mmol) and triphenylphosphine (138 mg, 0.53 mmol) were stirred in anhydrous THF and cooled to 0° C. DEAD (83 μl, 0.53 mmol) was added and the mixture was stirred at room temperature for 18 h. The mixture was filtered, diluted with EtOAc and washed with water and dried over sodium sulphate and concentrated in vacuo. The crude product was purified by flash chromatography eluting with EtOAc/hexane (4:1) to afford the title compound (11 mg).

1. filtrationThe mixture was filtered
2. additiondiluted with EtOAc
3. washwashed with water
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash chromatography
7. washeluting with EtOAc/hexane (4:1)