反应详情

温度

65 °C

N-{3-[3-(4-Methyl-benzo[b]thiophen-3-ylmethyl)-2-oxo-2,3-dihydro-benzimidazol-1-yl]-hexanoyl}-benzenesulfonamide (33 mg, 0.061 mmol) and Iodomethane (0.015 mL, 0.24 mmol) are added into DMF (1.0 mL) at room temperature. Then cesium carbonate (80 mg, 0.24 mmol) is added and the mixture is warmed up to 65° C. for 10 min. Then it is cooled down to room temperature for 16 hrs. Saturated NH4Cl solution (3.0 mL) and water (10 mL) are added and the mixture is extracted with EtOAc (3×20 mL). The organic layers are combined, dried (MgSO4) and concentrated to give crude product. Purification by flash column chromatography using EtOAc in hexanes (from 0% to 30%) affords 24 mg (71%) of N-Methyl-N-{3-[3-(4-methyl-benzo[b]thiophen-3-ylmethyl)-2-oxo-2,3-dihydro-benzimidazol-1-yl]-hexanoyl}-benzenesulfonamide. LCMS (ESMS): m/z 562.19 (M+H+).

1. temperatureThen it is cooled down to room temperature for 16 hrs
2. extractionthe mixture is extracted with EtOAc (3×20 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customto give crude product
6. customPurification by flash column chromatography