反应详情

温度

80 °C

2.94 g (12.41 mmol) of the compound from Example 81A and 2.50 g (11.28 mmol) of indium(III) chloride were added to 2.00 g (11.28 mmol) of the compound from Example 8 in 100 ml of toluene. The reaction mixture was stirred at 80° C. for 3 h. After cooling to RT, the reaction solution was mixed with water and ethyl acetate and the solid was filtered off. The phases of the filtrate were separated, and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. Purification of the crude product by preparative HPLC (mobile phase: acetonitrile/water gradient) resulted in 0.83 g (19% of theory) of the title compound.

1. temperatureAfter cooling to RT
2. filtrationthe solid was filtered off
3. customThe phases of the filtrate were separated
4. extractionthe aqueous phase was extracted with ethyl acetate
5. dry with materialThe combined organic phases were dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification of the crude product by preparative HPLC (mobile phase: acetonitrile/water gradient)