反应详情

In a 25 mL round-bottomed flask ethyl 6′-{[(ethylamino)carbonyl]amino}-4′-(4-phenyl-1,3-thiazol-2-yl)-3,3′-bipyridine-5-carboxylate (Example 131, 0.20 g, 0.42 mmol) was suspended in THF (3 mL). 1N LiOH (1.20 mL, 1.21 mmol) was added and the solution was stirred at room temperature over night. The solvent was removed and the resulting residue was diluted with water. The pH was adjusted to 4 (pH paper) with 2N HCl. White solids formed. They were trichurated with acetonitrile for 30 minutes and then filtered, washed with acetonitrile and dried in vacuo to give 58 mg of the title compound. LC/MS (ES+)[(M+H)+]: 446 for C23H11N5O3S. 1H NMR (300 MHz, d6-DMSO): 1.10 (t, 3H), 3.21 (m, 2H), 7.32-7.40 (m, 3H), 7.65 (t, 1H), 7.70 (s, 1H), 7.72 (s, 1H), 8.22 (s, 1H), 8.23-8.26 (m, 2H), 8.31 (s, 1H), 8.73 (d, 1H), 9.08 (d, 1H), 9.45 (s, 1H).

1. customThe solvent was removed
2. additionthe resulting residue was diluted with water
3. customWhite solids formed
4. filtrationfiltered
5. washwashed with acetonitrile
6. customdried in vacuo