Hydrochloric Acid → 5-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride

HRID 1765459

Reaktionsgleichung

Reaktionsgleichung von HRID 1765459
CO[CH:3](OC)[C:4](=[N:7][OH:8])[C:5]#[N:6].[OH:11][CH2:12][CH2:13][NH:14][NH2:15].[ClH:16]>CO>[ClH:16].[NH2:6][C:5]1[N:14]([CH2:13][CH2:12][OH:11])[N:15]=[CH:3][C:4]=1[N:7]=[O:8]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 80172-HydrazinoethanolHCID 713615623,3-Dimethoxy-2-hydroxyiminopropionitrile

Produkt 1

HCID 184268805-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochlorideAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
67 °C

Versuchsvorschrift

To a flask having an inner volume of 25 ml and equipped with a stirring device, a thermometer and a reflux condenser were charged 1.47 g (10.0 mmol) of 3,3-dimethoxy-2-hydroxyiminopropionitrile with a purity of 98.1% by weight synthesized in the same manner as in Example 1, 0.84 g (10.5 mmol) of 2-hydroxyethylhydrazine with a purity of 95% by weight, 10 ml of methanol and 1.5 ml (18.0 mmol) of conc. hydrochloric acid, and the mixture was reacted under reflux (67° C.) for 1.5 hours. After completion of the reaction, when the reaction mixture was analyzed by high performance liquid chromatography (absolute calibration curve method), it was found that 1.81 g of 5-amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride (Reaction yield: 93.8%) had been formed.

Aufarbeitung

  1. customTo a flask having
  2. customan inner volume of 25 ml and equipped with a stirring device
  3. customthe mixture was reacted
  4. customAfter completion of the reaction, when the reaction mixture

Quellen und Nachweise

ORD-Eintrag
ord-5181e8ae4bda4f58be10c7f24ccf6c1a
Quelldatensatz
uspto-grants-2007_06
Patentnummer
US07227032B2

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