HRID64170
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
PROCEDURE
实验过程
A solution of N-(5-(6-(6-(benzyloxy)pyridin-3-yl)-3H-imidazo[4,5-b]pyridin-3-yl)-2′,4′-difluoro-[1,1′-biphenyl]-3-yl)acetamide (0.10 g, 0.182 mmol) in TFA (4 ml) was stirred at RT for 16 h. The mixture was concentrated on vacuo, quenched with sodium bicarbonate and extracted as in Example 1(d). The solvent was distilled off to give the product in 84.3% yield (0.70 g)1H NMR (400 MHz, DMSO-d6): δ 10.42 (s, 1H), 8.98 (s, 1H), 8.68-8.67 (D, 1H), 8.43 (d, 1H), 8.31 (s, 1H), 7.99-7.96 (dd, 1H), 7.89 (s, 2H), 7.76-7.70 (m, 2H), 7.49-7.43 (m, 1H), 7.31-7.26 (m, 1H), 6.51-6.48 (d, 1H), 2.13 (s, 3H); LC-MS (ESI): Calculated mass 457.43: Observed mass: 458.1[M+H]+ (rt: 0.68 min).
WORKUP
后处理
- concentrationThe mixture was concentrated on vacuo
- customquenched with sodium bicarbonate
- extractionextracted as in Example 1(d)
- distillationThe solvent was distilled off
- customto give the product in 84.3% yield (0.70 g)1H NMR (400 MHz, DMSO-d6): δ 10.42 (s, 1H), 8.98 (s, 1H), 8.68-8.67 (D, 1H), 8.43 (d, 1H), 8.31 (s, 1H), 7.99-7.96 (dd, 1H), 7.89 (s, 2H), 7.76-7.70 (m, 2H), 7.49-7.43 (m, 1H), 7.31-7.26 (m, 1H), 6.51-6.48 (d, 1H), 2.13 (s, 3H)
- custom458.1[M+H]+ (rt: 0.68 min)