反应详情

温度

70 °C

In a sealed tube 3-(7-aminoimidazo[1,2-a]pyrimidin-2-yl)phenol hydrobromide (260 mg, 0.85 mmol) was combined in DMF (3 ml) to give a brown solution. Toluene-4-sulfonic acid fluoromethyl ester (249 mg, 1.22 mmol; CAS Nr. 114435-86-8) was dissolved in DMF and added. Cs2CO3 (527 mg, 1.62 mmol) was added. The reaction mixture was heated under argon to 70° C. for 9 h, then stirring was continued overnight at RT. The reaction mixture was diluted with H2O (30 ml) and extracted with EtOAc (3×30 ml). The combined organic layers were dried (MgSO4) and concentrated under vacuum and the crude product was purified by flash chromatography (50 g SiO2, DCM/MeOH/NH3aq. 140:10:1). The title compound (105 mg, 48%) was obtained as a yellow solid.

1. customto give a brown solution
2. additionadded
3. extractionextracted with EtOAc (3×30 ml)
4. dry with materialThe combined organic layers were dried (MgSO4)
5. concentrationconcentrated under vacuum
6. customthe crude product was purified by flash chromatography (50 g SiO2, DCM/MeOH/NH3aq. 140:10:1)