反应详情

10.0 g (47.7 mmol) of the compound from Example 3A and 8.3 g (57.1 mmol) of the compound from Example 7A are initially introduced into 100 ml ethanol and 1.5 ml (2.2 g, 19.0 mmol) TFA are added. The mixture is stirred under reflux for 12 h. A 4 M solution of hydrogen chloride in dioxane is then added in excess to the cooled reaction mixture, the mixture is extracted by stirring for approx. 1 h, the crystals which have precipitated out are filtered off and the residue on the filter is washed with dioxane and ethanol. The intermediate product obtained in this way is dissolved in 150 ml ethanol, 50 ml of a 25% strength methanolic sodium methylate solution are added and the mixture is stirred at RT for 2 h. The reaction mixture is then adjusted to pH 5 with 1 N hydrochloric acid and extracted by stirring at RT for a further 2 h, the solid is filtered off, the residue on the filter is washed with ethanol and the product is dried in vacuo.

1. additionare added
2. temperatureunder reflux for 12 h
3. customexcess to the cooled reaction mixture
4. extractionthe mixture is extracted
5. stirringby stirring for approx. 1 h
6. customthe crystals which have precipitated out
7. filtrationare filtered off
8. washthe residue on the filter is washed with dioxane and ethanol
9. customThe intermediate product obtained in this way
10. stirringthe mixture is stirred at RT for 2 h
11. extractionextracted
12. stirringby stirring at RT for a further 2 h
13. filtrationthe solid is filtered off
14. washthe residue on the filter is washed with ethanol
15. customthe product is dried in vacuo