反应详情

For 16 h, 2.8 g (19.6 mmol) of the compound from Example 7A and 4.3 g (19.6 mmol) of the compound from Example 3A are stirred in 50 ml of glacial acetic acid at boiling point (bath temperature 125° C.). For work-up, the resulting precipitate is filtered off, the filter residue is washed with diethyl ether and the filtrate is concentrated on a rotary evaporator. The filter residue is dissolved in 50 ml of ethanol, 18.5 ml (2.7 g, 39.2 mmol) of 21% strength ethanolic sodium methoxide solution are added and the solution is stirred at RT for 16 h. The reaction mixture is then adjusted to pH 5 using 1 N hydrochloric acid and stirred at RT for 2 h, the precipitate is then filtered off, the filter residue is washed with water and ethanol and the product is dried under reduced pressure.

1. filtrationFor work-up, the resulting precipitate is filtered off
2. washthe filter residue is washed with diethyl ether
3. concentrationthe filtrate is concentrated on a rotary evaporator
4. dissolutionThe filter residue is dissolved in 50 ml of ethanol
5. addition18.5 ml (2.7 g, 39.2 mmol) of 21% strength ethanolic sodium methoxide solution are added
6. stirringstirred at RT for 2 h
7. filtrationthe precipitate is then filtered off
8. washthe filter residue is washed with water and ethanol
9. customthe product is dried under reduced pressure