Methylhydrazine → 6-[5-(1-Imidazolylmethyl)-thien-2-yl]-2-methyl-3-oxo-2,3,4,5-tetrahydro-pyridazine

HRID 236275Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 236275
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][C:7]1[S:11][C:10]([C:12](=O)[CH2:13][CH2:14][C:15]([OH:17])=O)=[CH:9][CH:8]=1.[CH3:19][NH:20][NH2:21]>O>[NH:3]1[CH:4]=[CH:5][N:1]=[C:2]1[CH2:6][C:7]1[S:11][C:10]([C:12]2[CH2:13][CH2:14][C:15](=[O:17])[N:20]([CH3:19])[N:21]=2)=[CH:9][CH:8]=1

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 704292984-[5-(1-Imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid

Produkt 1

HCID 704292546-[5-(1-Imidazolylmethyl)-thien-2-yl]-2-methyl-3-oxo-2,3,4,5-tetrahydro-pyridazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 8.7 g of 4-[5-(1-imidazolylmethyl)-thien-2-yl]-4-oxobutyric acid, 2.9 ml methylhydrazine and 100 ml water was heated at 90° C. for 2 hours. After cooling, the precipitated solid was filtered off, dissolved in chloroform, the chloroform phase washed with dilute caustic soda solution and with water, dried over sodium sulfate and evaporated. The residue was purified by column chromatography (Silica gel//chloroform) and finally recrystallized from ethanol.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe precipitated solid was filtered off
  3. dissolutiondissolved in chloroform
  4. washthe chloroform phase washed with dilute caustic soda solution and with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was purified by column chromatography (Silica gel//chloroform)
  8. customfinally recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-facaa37b75c84a20a64edf600cdada5b
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04643998

Notizen zur Reaktion

Wird geladen…