Reaktion #614497

Reaktionsgleichung

hydrazine hydrate

4-(4-aminophenyl)morpholin-3-one

2-cyano-3,3-bis(methylthio)acrylamide

→

5-amino-3-((4-(2-oxomorpholino)phenyl)amino)-1H-pyrazole-4-carboxamide

Lösungsmittel

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigereaction at 75° C.
2. 2
   SonstigeOnce complete (18 hrs), reaction
3. 3
   Sonstigewas brought to room temperature
4. 4
   Filtrationfiltered
5. 5
   Sonstigeto obtain a light yellow powder as product
6. 6
   Sonstigeto dry under vacuum for 1 hr
7. 7
   SonstigeReaction
8. 8
   Sonstige(18 hrs), reaction
9. 9
   Sonstigewas brought to room temperature
10. 10
    Filtrationfiltered

Vorschrift

Dissolved 0.500 g 2-cyano-3,3-bis(methylthio)acrylamide in 15 mL EtOH and added 4-(4-aminophenyl)morpholin-3-one (1.0 eq.). Stirred reaction at 75° C. until starting amide was absent by HPLC. Once complete (18 hrs), reaction was brought to room temperature and filtered to obtain a light yellow powder as product. Product was allowed to dry under vacuum for 1 hr. Product was then suspended in 10 mL EtOH and hydrazine hydrate (1 eq.) was added dropwise. Reaction was heated at 75° C. until intermediate was absent (HPLC). Once intermediate was absent (18 hrs), reaction was brought to room temperature and filtered to obtain 5-amino-3-((4-(2-oxomorpholino)phenyl)amino)-1H-pyrazole-4-carboxamide as a yellow powder. Product was allowed to dry under vacuum for 1 hr.

Quelle