Water → 3-amino-1-phenyl-1H-pyrazole-4-carboxamide

HRID 1961501

Reaktionsgleichung

Reaktionsgleichung von HRID 1961501
[NH2:1][C:2]1[C:6]([C:7]#[N:8])=[CH:5][N:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.[OH2:15]>OS(O)(=O)=O>[NH2:1][C:2]1[C:6]([C:7]([NH2:8])=[O:15])=[CH:5][N:4]([C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:3]=1

Komponenten

4

Edukt 2

HCID 962WaterHCID 27742493-Amino-1-phenyl-1H-pyrazole-4-carbonitrile

Produkt 1

HCID 88319093-amino-1-phenyl-1H-pyrazole-4-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Versuchsvorschrift

3-amino-1-phenyl-1H-pyrazole-4-carbonitrile (0.34 g, 1.846 mmol) was stirred in 95% H2SO4 (10 mL) at 50° C. for 3 hours. Room temperature was attained, water was added and the products extracted into EtOAc (×3). The aqueous phase was neutralised with 2 N NaOH and the products extracted into DCM (×2) followed by 20% MeOH-DCM (×4). The combined organic extracts were dried over MgSO4 and concentrated in vacuo. The residue was triturated in EtOAc to give 3-amino-1-phenyl-1H-pyrazole-4-carboxamide as a pale yellow solid.

Aufarbeitung

  1. customRoom temperature
  2. extractionthe products extracted into EtOAc (×3)
  3. extractionthe products extracted into DCM (×2)
  4. dry with materialThe combined organic extracts were dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was triturated in EtOAc

Quellen und Nachweise

ORD-Eintrag
ord-88b0fe6ae8224b3cbc7ca4ae5867fb06
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08415346B2

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