Reaktion #816423

Reaktionsgleichung

hydrochloric acid

dioxane

5-tert-butyl 1-ethyl 3-{[4-(4-methylpiperazin-1-yl)benzoyl]amino}-4,6-dihydropyrrolo[3,4-c]pyrazole-1,5-dicarboxylate

→

title compound

ethyl 3-{[4-(4-methylpiperazin-1-yl)benzoyl]amino}-5,6-dihydropyrrolo[3,4-c]pyrazole-1(4H)-carboxylate trihydrochloride

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprecipitation of a white solid
2. 2
   Filtrationafter dilution with Et20 (100 ml), the solid was filtered
3. 3
   Waschenextensively washed with Et20
4. 4
   Sonstigedried under vacuum at 50° C.

Vorschrift

A 4N solution of hydrochloric acid in dioxane (122 ml, 488 mmol) was added dropwise to a stirred solution of 5-tert-butyl 1-ethyl 3-{[4-(4-methylpiperazin-1-yl)benzoyl]amino}-4,6-dihydropyrrolo[3,4-c]pyrazole-1,5-dicarboxylate (19.5 g, 39.2 mmol), as prepared in Example 2, in dry DCM (240 ml); precipitation of a white solid occurred almost immediately. The resulting mixture was stirred at room temperature for 24 hours; after dilution with Et20 (100 ml), the solid was filtered, extensively washed with Et20, and dried under vacuum at 50° C. to give 20.1 g of the title compound, used in the next step without further purification. [M+H]+ 399.

Quelle