反应详情

10.0 g (47.8 mmol) of the compound from Example 42A and 8.3 g (57.3 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. The crystals which have precipitated out are filtered off, the residue on the filter is rinsed with ethanol and the intermediate product is dried overnight in vacuo. This is then suspended in 20 ml methanol, 100 ml of a 4 M solution of hydrogen chloride in dioxane are added and the mixture is subsequently stirred at RT for 1 h. The solid is filtered off, the residue on the filter is washed with dioxane, ethyl acetate and diisopropyl ether and the product is dried in vacuo.

1. additionare added
2. temperatureunder reflux for 12 h
3. customThe crystals which have precipitated out
4. filtrationare filtered off
5. washthe residue on the filter is rinsed with ethanol
6. customthe intermediate product is dried overnight in vacuo
7. addition100 ml of a 4 M solution of hydrogen chloride in dioxane are added
8. stirringthe mixture is subsequently stirred at RT for 1 h
9. filtrationThe solid is filtered off
10. washthe residue on the filter is washed with dioxane, ethyl acetate and diisopropyl ether
11. customthe product is dried in vacuo