反应详情

A solution of the amine of Example 43 (98 mg, 0.30 mmol) in dimethylformamide (3.75 ml) was treated with 1-methylimidazole-4-sulphonyl chloride (60 mg, 0.33 mmol) and triethylamine (46 μL, 0.33 mmol) and the resulting mixture was stirred at room temperature for 18 hours. The solution was concentrated under reduced pressure. The residue was partitioned between dichloromethane and saturated aqueous sodium hydrogencarbonate solution. The organic extract was dried over anhydrous magnesium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by flash chromatography on silica gel eluting with dichloromethane:methanol (95:5, by volume) to afford the title compound (55 mg) as a white solid, m.p. 172–174° C.

1. concentrationThe solution was concentrated under reduced pressure
2. customThe residue was partitioned between dichloromethane and saturated aqueous sodium hydrogencarbonate solution
3. extractionThe organic extract
4. dry with materialwas dried over anhydrous magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by flash chromatography on silica gel eluting with dichloromethane:methanol (95:5, by volume)