反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 45 °C
PROCEDURE
实验过程
Ethyl 6′-{[(ethylamino)carbonyl]amino}-5″-fluoro-3,3′:4′,3″-terpyridine-5-carboxylate (Example 68, 0.19 g, 0.46 mmol) was added to a 25 mL round-bottomed flask with THF (3 mL) to give a white suspension. Lithium hydroxide (1.160 mL, 1.16 mmol) was added to the mixture, and the solution was stirred at 45° C. for 2 h. The solvent was removed under reduced pressure, and the resulting residue was diluted with water and adjusted to pH˜4 by 2N HCl. The precipitate that formed was collected by filtration, washed with water, and dried to give the title compound as a white solid (154 mg). MS (ESP): 382 (MH+) for C19H16FN5O3; NMR: 1.08 (t, 3H), 3.13-3.24 (m, 2H), 7.63 (s, 1H) 7.64-7.68 (m, 1H) 7.69-7.77 (m, 1H), 7.93 (t, 1H), 8.19 (t, 1H), 8.36 (s, 1H), 8.45 (d, 1H), 8.55 (d, 1H), 8.90 (d, 1H), 9.45 (s, 1H).
WORKUP
后处理
- customto give a white suspension
- customThe solvent was removed under reduced pressure
- additionthe resulting residue was diluted with water
- customThe precipitate that formed
- filtrationwas collected by filtration
- washwashed with water
- customdried