反应详情

温度

50 °C

To a suspension of 2,3-dibromothieno[2,3-c]pyridine (400 mg, 1.37 mmol), 2-methyl-3-butyn-2-ol (121 μL, 1.24 mmol), copper (I) iodide (24 mg, 0.12 mmol) and DIPEA (2.16 mL, 12.41 mmol) in 1,4-dioxane (16 mL) was added Pd(PPh3)2Cl2 (174 mg, 0.25 mmol). The mixture was evacuated and refilled with nitrogen (3×), then stirred at 50° C. for 2 h. Solvent was evaporated and the resultant mixture was dissolved in EtOAc. The organic solution was washed with water and brine, dried over anhydrous sodium sulfate, and purified by ISCO column chromatography (0 to 5% MeOH:DCM) to afford 319 mg (87%) of the title compound as a light-yellow solid. MS (ESI): 296.38, 298.35 [M+H]+; HPLC tR=0.94 min (HPLC: Analytical—2 min).

1. customThe mixture was evacuated
2. additionrefilled with nitrogen (3×)
3. customSolvent was evaporated
4. dissolutionthe resultant mixture was dissolved in EtOAc
5. washThe organic solution was washed with water and brine
6. dry with materialdried over anhydrous sodium sulfate
7. custompurified by ISCO column chromatography (0 to 5% MeOH:DCM)