反应详情

温度

120 °C

3.45 g (40.1 mmoles) of piperazine is placed in the presence of 1.7 g (13.4 mmoles) of intermediate 2a in 1-butanol. 6.5 ml (47 mmoles) of triethylamine is added and the mixture is heated for 24 hours at 120° C. After concentrating the reaction medium, the residue obtained is taken up with ethyl acetate and washed with water. After drying on MgSC4, the organic phase is concentrated to dryness. The residue obtained is purified by flash chromatography (CH2Cl2-MeOH-NH4OH gradient: 100-0-0 to 90-9-1). 1.52 g of intermediate 5a is obtained in brown oil form (yield: 69%).

1. concentrationAfter concentrating the reaction medium
2. customthe residue obtained
3. washwashed with water
4. customAfter drying on MgSC4
5. concentrationthe organic phase is concentrated to dryness
6. customThe residue obtained
7. customis purified by flash chromatography (CH2Cl2-MeOH-NH4OH gradient: 100-0-0 to 90-9-1)