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Hydrazine → tert-Butyl 4,6-dihydropyrrolo(3,4-c)pyrazole-5(1H)-carboxylate

HRID 241560
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 241560
[NH2:1]N.C[N:4](/[CH:6]=[C:7]1/[CH2:8][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:10][C:11]/1=O)C>C(O)C>[NH:1]1[C:11]2[CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8][C:7]=2[CH:6]=[N:4]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 9321HydrazineHCID 56971730(Z)-tert-butyl 3-((dimethylamino)methylene)-4-oxopyrrolidine-1-carboxylate

Produkt 1

HCID 7147072tert-Butyl 4,6-dihydropyrrolo(3,4-c)pyrazole-5(1H)-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of hydrazine (3 mL) and tert-butyl (3Z)-3-[(dimethylamino)methylene]-4-oxopyrrolidine-1-carboxylate (19.22 g) in ethanol (40 mL) was heated at 85° C. in a sealed tube for 4 h. Solvent was removed under reduced pressure, and the residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL). The resulting solid was filtered. The filtrate was concentrated and the resulting solid was triturated again. The combined solids were used in the next step.

Aufarbeitung

  1. customSolvent was removed under reduced pressure
  2. customthe residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL)
  3. filtrationThe resulting solid was filtered
  4. concentrationThe filtrate was concentrated
  5. customthe resulting solid was triturated again

Quellen und Nachweise

ORD-Eintrag
ord-fd4c7b181d984b04853f1342e9f2316a
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08653059B2

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