反应详情

温度

24 °C

5-fluoroskatole (670 mg, 4.49 mmol) together with 2-(2-(2-(4-butyl-4-dimethylaminocyclohex-1-enyl)-1H-indol-3-yl)-ethyl)isoindol-1,3-dione (700 mg, 1.49 mmol) was dissolved in abs. dichloromethane (5 ml) and mixed with trifluoromethane sulphonic acid (0.175 ml, 1.974 mmol). The batch was stirred for 10 d at 24° C. The precipitated light beige-coloured solid was separated by filtration and washed with dichloromethane (3×0.5 ml). The solid (1031 mg) was stirred for 10 min with 1N sodium hydroxide solution (20 ml) and dichloromethane (20 ml). The phases were separated. The aqueous phase was extracted with dichloromethane (2×20 ml). The combined organic extracts were dried over Na2SO4 and then concentrated to low volume. The product was purified by column chromatography.

1. customThe precipitated light beige-coloured solid was separated by filtration
2. washwashed with dichloromethane (3×0.5 ml)
3. stirringThe solid (1031 mg) was stirred for 10 min with 1N sodium hydroxide solution (20 ml) and dichloromethane (20 ml)
4. customThe phases were separated
5. extractionThe aqueous phase was extracted with dichloromethane (2×20 ml)
6. dry with materialThe combined organic extracts were dried over Na2SO4
7. concentrationconcentrated to low volume
8. customThe product was purified by column chromatography