反应详情

温度

110 °C

4.75 g (55.15 mmol) of piperazine are placed in the presence of 4.05 g (18.4 mmol) of intermediate 1b in toluene at room temperature for 30 min. 2.8 mL (20.1 mmol) of triethylamine are added and the mixture is heated for 18 h at 110° C. After concentration of the reaction medium, the obtained residue is taken up with dichloromethane and washed with water. After drying on MgSO4, the organic phase is dry concentrated. The obtained residue is purified by flash chromatography (CH2Cl2-MeOH: 60-40). 3.3 g of intermediate 12a is obtained as a white powder (yield: 79%).

1. washwashed with water
2. customAfter drying on MgSO4
3. customthe organic phase is dry
4. concentrationconcentrated
5. customThe obtained residue is purified by flash chromatography (CH2Cl2-MeOH: 60-40)