反应详情

Triethylamine (0.28 ml, 2.04 mmol) was added in one portion to a stirred solution of N-[4-(piperazine-1-sulfonyl)-phenyl]-acrylamide (0.2 g, 0.68 mmol) and 3-pyridine propionic acid (0.1 g, 0.68 mmol) in THF (5 ml). The mixture was stirred at room temperature for 5 minutes before EDC (0.26 g, 1.36 mmol) was added in one portion and the resulting mixture and stirred at room temperature under a nitrogen atmosphere for 18 hours. The crude reaction mixture was concentrated under vacuum and the resulting residue dissolved in DCM (20 ml), washed with water (20 ml), dried (MgSO4), filtered and concentrated under vacuum. The crude product was purified by Prep HPLC to give the title compound (0.046 g, 15% yield) as a white powder.

1. additionwas added in one portion
2. customThe crude reaction mixture
3. concentrationwas concentrated under vacuum
4. dissolutionthe resulting residue dissolved in DCM (20 ml)
5. washwashed with water (20 ml)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customThe crude product was purified by Prep HPLC