反应详情

温度

200 °C

A mixture of 4-amino-2-bromo-3,6-dimethylthieno[2,3-b]pyridine-5-carboxylic acid (Description 61) (720 mg, 2.391 mmol) and diphenyl ether (3.80 mL, 23.91 mmol) was heated to 200° C. for 48 h. The mixture was then cooled to RT, taken-up in MeOH (10 mL) and purified on silica, eluting with a gradient of 0-20% 2M NH3 in MeOH in DCM. Further purification by SCX, eluting with 0-100% 2M NH3 in MeOH in MeOH afforded the title compound (350 mg). LCMS (A) m/z: 257/259 [M+1]+, Rt 1.10 min (basic).

1. custompurified on silica
2. washeluting with a gradient of 0-20% 2M NH3 in MeOH in DCM
3. customFurther purification by SCX
4. washeluting with 0-100% 2M NH3 in MeOH in MeOH