反应详情

温度

120 °C

Into a 150 mL sealed tube was placed a solution of 1-acetyl-1H-indol-3-yl acetate (2.5 g, 11.51 mmol) in toluene (80 mL). To this was added tert-butyl piperazine-1-carboxylate (10.71 g, 57.55 mmol). To the mixture was added p-toluenesulfonic acid (400 mg, 2.33 mmol). The resulting solution was allowed to react, with stirring, overnight while the temperature was maintained at 120° C. in a bath of oil. The reaction progress was monitored by TLC (ethyl acetate/petroleum ether=1:1). The mixture was concentrated by evaporation under vacuum using a rotary evaporator. The resulting solution was diluted with 200 mL of ethyl acetate. The resulting mixture was washed 3 times with 200 mL of NaCl(aq.). The mixture was dried over Na2SO4. The residue was purified by eluting through a column with a 10:1 petroleum ether/ethyl acetate solvent system. This resulted in 2.9 g (72%) of tert-butyl 4-(1-acetyl-1H-indol-3-yl)piperazine-1-carboxylate as a purple solid.

1. customInto a 150 mL sealed tube
2. customto react
3. concentrationThe mixture was concentrated by evaporation under vacuum
4. customa rotary evaporator
5. additionThe resulting solution was diluted with 200 mL of ethyl acetate
6. washThe resulting mixture was washed 3 times with 200 mL of NaCl(aq.)
7. dry with materialThe mixture was dried over Na2SO4
8. customThe residue was purified
9. washby eluting through a column with a 10:1 petroleum ether/ethyl acetate solvent system
10. customThis resulted in 2.9 g (72%) of tert-butyl 4-(1-acetyl-1H-indol-3-yl)piperazine-1-carboxylate as a purple solid