Methylhydrazine → 5-Amino-1-methyl-4-nitroso-3-phenylpyrazole

HRID 1085159Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1085159
[OH:1][N:2]=[C:3]([C:6](=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[C:4]#[N:5].[CH3:14][NH:15][NH2:16]>C(O)C>[NH2:5][C:4]1[N:15]([CH3:14])[N:16]=[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:3]=1[N:2]=[O:1]

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 85446889HCID 85446889, Verbindung

Produkt 1

HCID 53253435-Amino-1-methyl-4-nitroso-3-phenylpyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 2-hydroxyimino-3-oxo-3-phenylpropanenitrile (2.61 g, 15 mmol) and methylhydrazine (1.1 ml, 21 mmol) was stirred at reflux in ethanol (20 ml) for 2 hours, cooled and concentrated under reduced pressure. The residue was partitioned between ether (50 ml) and dilute hydrochloric acid (50 ml, 2N solution). The aqueous phase was separated and rendered basic by the addition of saturated aqueous potassium carbonate. The red solid which precipitated was filtered off and dried, to give the title compound, 1.40 g, (46%). m.p. 230°-231° C. (literature. m.p. 230°-231° C., Gazz. Chim. Ital., (1968), 98, 569.

Aufarbeitung

  1. temperaturecooled
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was partitioned between ether (50 ml) and dilute hydrochloric acid (50 ml, 2N solution)
  4. customThe aqueous phase was separated
  5. additionrendered basic by the addition of saturated aqueous potassium carbonate
  6. customThe red solid which precipitated
  7. filtrationwas filtered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-15125575561b426caee623cc83c08b6c
Quelldatensatz
uspto-grants-1991_04
Patentnummer
US05008263

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