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
- 0 °C
PROCEDURE
实验过程
A solution of methyl 4-(8-(3-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridine-2-ylamino)benzoate (1.03 g, 2.50 mmol, 1 equiv) in 2M aqueous sodium hydroxide (10 mL) and 1,4-dioxane (5 mL) was heated at 80-90° C. After 3 h, the solution was cooled to 0° C. and neutralized by the addition of 6M HCl until pH=4-5. The resulting solid was collected by filtration and rinsed sequentially with water, isopropanol, and hexanes to afford crude 4-(8-(3-(trifluoromethyl)phenyl)-[1,2,4]triazolo[1,5-a]pyridin-2-ylamino)benzoic acid (1.0 g, HPLC purity: 89%). LCMS (ESI) m/z: 398.9; 1H NMR (400 MHz, DMSO-d6) δ: 12.45 (br s, 1 H), 10.22 (s, 1 H), 8.89 (d, J=6.8 Hz, 1 H), 8.65 (s, 1 H), 8.42 (d, J=6.9 Hz, 1 H), 8.03 (m, 1 H), 7.77-7.84 (m, 6 H), 7.21 (t, J=7.0 Hz, 1 H).
WORKUP
后处理
- filtrationThe resulting solid was collected by filtration
- washrinsed sequentially with water, isopropanol, and hexanes