反应详情

温度

100 °C

To a 250 mL flask were added trimethylbenz[e]indole (5.21 g, 24.9 mmol), acetonitrile (80 mL) and 6-iodohexanoic acid (6.5 g, 26.9 mmol). The mixture was heated at reflux under argon for 1 h and then approx. 70 mL of the acetonitrile was removed by distillation. The mixture was heated at 100° C. for 20 h. The green mixture of solid and liquid was cooled to rt and the volatile components were removed in vacuo. The residue was triturated with ether (2×60 mL), ethyl acetate (2×60 mL) and with ether (2×60 mL) to give 12 as a powder (8.51 g, 75%).

1. temperatureThe mixture was heated
2. temperatureat reflux under argon for 1 h
3. customapprox. 70 mL of the acetonitrile was removed by distillation
4. additionThe green mixture of solid and liquid
5. temperaturewas cooled to rt
6. customthe volatile components were removed in vacuo
7. customThe residue was triturated with ether (2×60 mL), ethyl acetate (2×60 mL) and with ether (2×60 mL)