反应详情

温度

60 °C

1-{5-[7-Bromo-2-(3-ethyl-ureido)-benzothiazol-5-yl]-pyrimidin-2-yl}-4-methyl-piperidine-4-carboxylic acid (16 mg) was dissolved in EtOH (5 mL), THF (1 mL) and AcOH (0.5 mL) and 10% palladium on carbon (3 mg) was added followed by ammonium formate (78 mg). The mixture was degassed and heated at 60° C. for four days then cooled to rt. The mixture was filtered through a syringe filter and the filtrate concentrated in vacuo. The material was purified by preperative HPLC (Gilson, 40-60%, water/MeCN+0.1% formic acid). The relevant fractions were combined and freeze-dried overnight to give Compound 46 as a white solid (5.2 mg). 1H NMR ((CD3)2SO): δ 1.09 (3H, t, J=7.2 Hz), 1.13 (3H, s), 1.29 (2H, m), 2.03 (2H, br d, J=13.5 Hz), 3.17 (4H, m), 4.1 (1H, br s), 4.23 (2H, br dt, J=13.5 and 4.7 Hz), 7.43 (1H, dd, J=8.2 and 1.5 Hz), 7.6 (1H, br s), 7.83 (1H, d, J=1.5 Hz), 7.88 (1H, d, J=8.2 Hz), 8.71 (2H, s), 11.5 (1H, br s). m/z: 441 [M+H]+.

1. customThe mixture was degassed
2. temperaturethen cooled to rt
3. filtrationThe mixture was filtered through a syringe
4. filtrationfilter
5. concentrationthe filtrate concentrated in vacuo
6. customThe material was purified by preperative HPLC (Gilson, 40-60%, water/MeCN+0.1% formic acid)
7. customfreeze-dried overnight