反应详情

Into a 250 mL round bottom flask was placed a solution of tert-butyl 4-(1-acetyl-1H-indol-3-yl)piperazine-1-carboxylate (2.6 g, 7.58 mmol) in methanol (80 mL). To the mixture was added Et3N (2.3 g, 22.73 mmol). The resulting solution was allowed to react, with stirring, for 1 hour while the temperature was maintained at reflux in a bath of oil. The reaction progress was monitored by LCMS and 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 150 mL of NaCl(aq.). The residue was purified by eluting through a column with a 10:1 petroleum ether/ethyl acetate solvent system. This resulted in 2.1 g (89%) of tert-butyl 4-(1H-indol-3-yl)piperazine-1-carboxylate as a light pink solid.

1. customInto a 250 mL round bottom flask was placed
2. customto react
3. temperaturewas maintained
4. temperatureat reflux in a bath of oil
5. concentrationThe mixture was concentrated by evaporation under vacuum
6. customa rotary evaporator
7. additionThe resulting solution was diluted with 200 mL of ethyl acetate
8. washThe resulting mixture was washed 3 times with 150 mL of NaCl(aq.)
9. customThe residue was purified
10. washby eluting through a column with a 10:1 petroleum ether/ethyl acetate solvent system
11. customThis resulted in 2.1 g (89%) of tert-butyl 4-(1H-indol-3-yl)piperazine-1-carboxylate as a light pink solid