HRID1676238
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Prepared from ethyl 2-(3-fluoro-4-(thieno[3,2-b]pyridin-7-yloxy)phenylamino)-2-oxoacetate (Example 2; 36 mg, 0.10 mmol) and 3-fluoroaniline (139 mg, 1.25 mmol) according to the procedure for Example 3, except the reaction was heated to 100° C. for 18 hours. The product was purified by preparative TLC (1:1 EtOAc/hexanes). The product was obtained as a white powder (7 mg, 6%). 1H NMR (400 MHz, CDCl3+MeOD-d3) δ 8.48 (d, J=6 Hz, 1H), 7.92 (m, 1H), 7.83 (d, J=6 Hz, 1H), 7.67 (m, 1H), 7.57 (d, J=6 Hz, 1H), 7.51 (m, 1H), 7.35 (m, 3H), 6.94 (m, 1H), 6.57 (d, J=6 Hz, 1H). LRMS (ESI pos) m/e 426 (M+1). HPLC: 97% purity (220 nm).
WORKUP
后处理
- customThe product was purified by preparative TLC (1:1 EtOAc/hexanes)