反应详情

12.8 g (70.27 mmol) of 5-hydroxy-3-isopropyl-indole are dissolved in 275.8 ml of DMSO, 10.68 g (77.3 mmol) of potassium carbonate are introduced in solid form, the mixture is stirred for 10 minutes at room temperature and afterwards 19.43 g (70.27 mmol) of 3,5-bistrifluoromethyl-4-chlorobenzaldehyde are introduced in portions. After stirring at 50° C. for 3 hours the batch is poured onto a mixture of 400 ml of ethyl acetate and 250 ml of saturated ammonium chloride solution. After phase separation, the aqueous phase is extracted again with ethyl acetate, and the combined organic phases are washed twice with sodium chloride solution and dried over sodium sulphate. After removing the drying agent and distilling off the solvent the crude product is chromatographed on silica gel 60 (Merck 0.040-0.063 mm) using toluene.

1. stirringAfter stirring at 50° C. for 3 hours the batch
2. customAfter phase separation
3. extractionthe aqueous phase is extracted again with ethyl acetate
4. washthe combined organic phases are washed twice with sodium chloride solution
5. dry with materialdried over sodium sulphate
6. customAfter removing the drying agent
7. distillationdistilling off the solvent the crude product
8. customis chromatographed on silica gel 60 (Merck 0.040-0.063 mm)