反应详情

To a yellow solution mixture of 3-(4-fluoro-2-(4-fluorophenyl)-3-(methylcarbamoyl)benzofuran-5-yl)-4-methylbenzoic acid (30 mg, 0.071 mmol) and 3-(pyrimidin-2-yl)oxetan-3-amine hydrochloride (16 mg, 0.085 mmol) in DMF (1 ml) in a 25 ml round-bottomed flask was added benzotriazo-1-yloxytripyrrolidinophosphonium hexafluorophosphate (PyBOP) (50 mg, 0.096 mmol), followed by triethylamine (TEA) (0.1 ml, 0.717 mmol), and the reaction mixture stirred for overnight. Ice cooled water was added to the reaction mixture, which was then stirred for 10-15 min. at 0° C. Precipitation was observed. The solid was collected by filtration, washed with cold water, and then dissolved in dichloromethane. The organic was dried over Na2SO4, filtered and concentrated. The crude product was purified by preparative HPLC. Yield (12 mg, 30%).

1. additionwas added to the reaction mixture, which
2. stirringwas then stirred for 10-15 min. at 0° C
3. customPrecipitation
4. filtrationThe solid was collected by filtration
5. washwashed with cold water
6. dissolutiondissolved in dichloromethane
7. dry with materialThe organic was dried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude product was purified by preparative HPLC
11. customYield (12 mg, 30%)