反应详情

温度

100 °C

1.1 ml (1.6 g, 13.8 mmol) TFA are added to a mixture of 7.3 g (34.6 mmol) of the compound from Example 3A and 6.0 g (41.5 mmol) of the compound from Example 7A in 70 ml ethanol and the mixture is stirred at 100° C. for 20 h. The solid which has precipitated out is filtered off and the filtrate is concentrated in vacuo. The residue is suspended in 100 ml ethanol, 30 ml of a 30% strength sodium methanolate solution in methanol are added and the mixture is stirred at RT for 1.5 h. After addition of 42 ml of a 4 N solution of hydrogen chloride in dioxane (pH=5-6) and after stirring for 30 min, the solid is filtered off, washed first with ethanol and then with diethyl ether and dried in vacuo. Further purification is carried out by stirring in ethanol and acetonitrile several times. 10 ml of a 4 N solution of hydrogen chloride in dioxane are then added and the mixture is stirred at RT for 16 h. The product is filtered off, washed first with acetonitrile and then with diethyl ether and dried in vacuo.

1. customThe solid which has precipitated out
2. filtrationis filtered off
3. concentrationthe filtrate is concentrated in vacuo
4. addition30 ml of a 30% strength sodium methanolate solution in methanol are added
5. stirringthe mixture is stirred at RT for 1.5 h
6. additionAfter addition of 42 ml of a 4 N solution of hydrogen chloride in dioxane (pH=5-6)
7. stirringafter stirring for 30 min
8. filtrationthe solid is filtered off
9. washwashed first with ethanol
10. dry with materialwith diethyl ether and dried in vacuo
11. customFurther purification
12. stirringby stirring in ethanol
13. addition10 ml of a 4 N solution of hydrogen chloride in dioxane are then added
14. stirringthe mixture is stirred at RT for 16 h
15. filtrationThe product is filtered off
16. washwashed first with acetonitrile
17. dry with materialwith diethyl ether and dried in vacuo