反应详情

温度

10 °C

Batch 2: A further amount of the title compound is obtained as follows: The residue (2.4 g) obtained from the mother liquor during the synthesis of Example Compound 71, which contains the open-ring intermediate state of the cyclization, 3-[2-(6-morpholin-4-ylpyrimidin-4-yl)hydrazino]-2-(1H-1,2,3-triazol-1-yl)prop-2-enoic acid ethyl ester, is dissolved in 12 ml ethanol and 1.5 ml 30% strength sodium methylate solution in methanol are added at RT, while stirring. The mixture is subsequently stirred at RT for 45 min, then adjusted to pH 5 with 2 N hydrochloric acid and subsequently stirred at RT for a further 16 h. The mixture is cooled to 10° C. and the solid is filtered off and washed with 3.5 ml dioxane. The mixture is dried under a high vacuum for 16 h, 5 ml methanol are then added and the mixture is subsequently stirred at RT for 1 h. The solid is filtered off, washed with 2 ml methanol and dried under a high vacuum to give a further 997 mg of the title compound in this way.

1. stirringThe mixture is subsequently stirred at RT for 45 min
2. stirringsubsequently stirred at RT for a further 16 h
3. filtrationthe solid is filtered off
4. washwashed with 3.5 ml dioxane
5. customThe mixture is dried under a high vacuum for 16 h
6. addition5 ml methanol are then added
7. stirringthe mixture is subsequently stirred at RT for 1 h
8. filtrationThe solid is filtered off
9. washwashed with 2 ml methanol
10. customdried under a high vacuum