反应详情

24 mg (0.07 mmol) of cesium carbonate were added to a solution of 58 mg of tert-butyl {3-[6-amino-1-(3-methylbut-2-enyl)-1H-benzimidazol-2-ylsulfanyl]propyl}carbamate (obtained analogously to examples 1a-c) in 5 ml of dimethylformamide, and the mixture was stirred at room temperature for 30 minutes. Subsequently, 17 μl (0.15 mmol) of benzoyl bromide were added and the mixture was stirred at room temperature for 20 hours. The reaction mixture was concentrated under reduced pressure and partitioned between water and dichloromethane. The organic phase was dried, concentrated under reduced pressure and purified by means of preparative HPLC (acetonitrile/water+0.5% trifluoroacetic acid, gradient: 20/80 to 100/0). 33 mg (44%) of the desired product were obtained.

1. stirringthe mixture was stirred at room temperature for 20 hours
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. custompartitioned between water and dichloromethane
4. customThe organic phase was dried
5. concentrationconcentrated under reduced pressure
6. custompurified by means of preparative HPLC (acetonitrile/water+0.5% trifluoroacetic acid, gradient: 20/80 to 100/0)