Hydrochloric Acid → 2-Pyridin-2-yl-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

HRID 889306Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 889306
C([O:3][C:4](=O)[CH:5]([C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)[CH:6]=[N:7][NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)C.C([O-])C.[Na+].Cl>C(O)C>[N:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[N:8]1[C:4](=[O:3])[C:5]([C:15]2[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=2)=[CH:6][NH:7]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 2723922Sodium ethoxideHCID 687052862-Pyridin-3-yl-3-(pyridin-2-ylhydrazono)propionic acid ethyl ester

Produkt 1

HCID 591869472-Pyridin-2-yl-4-pyridin-3-yl-1,2-dihydro-3H-pyrazol-3-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

3.95 g (13.9 mmol) of the compound from Example 3A are initially introduced into 80 ml ethanol under argon and 945 mg (13.9 mmol) sodium ethanolate are added in portions at RT. After stirring for 30 min, 13.9 ml 1 M hydrochloric acid are added dropwise. The precipitate which has separated out is filtered off with suction, washed with cold ethanol (20 ml) and with water (twice with 20 ml each time) and dried in vacuo. 2.80 g (85% of th.) of the title compound are obtained.

Aufarbeitung

  1. customThe precipitate which has separated out
  2. filtrationis filtered off with suction
  3. washwashed with cold ethanol (20 ml) and with water (twice with 20 ml each time) and
  4. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-ef843123af2949c3a892d2f4d595be26
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08252817B2

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