N,N-Dimethylglycine hydrazide hydrochloride → 2,6-Diacetylpyridine bis(dimethylaminoacetylhydrazone) dihydrochloride

HRID 2120092

Reaktionsgleichung

Reaktionsgleichung von HRID 2120092
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10](=O)[CH3:11])[N:5]=1)(=O)[CH3:2].[ClH:13].[CH3:14][N:15]([CH2:17][C:18]([NH:20][NH2:21])=[O:19])[CH3:16]>C(O)C.O.C(O)(C)C>[ClH:13].[ClH:13].[CH3:14][N:15]([CH2:17][C:18]([NH:20][N:21]=[C:1]([C:4]1[N:5]=[C:6]([C:10](=[N:21][NH:20][C:18](=[O:19])[CH2:17][N:15]([CH3:16])[CH3:14])[CH3:11])[CH:7]=[CH:8][CH:9]=1)[CH3:2])=[O:19])[CH3:16]

Komponenten

6

Edukt 2

HCID 68318N,N-Dimethylglycine hydrazide hydrochlorideHCID 707902,6-Diacetylpyridine

Produkt 1

HCID 765297142,6-Diacetylpyridine bis(dimethylaminoacetylhydrazone) dihydrochlorideAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A solution of 2,6-diacetylpyridine (Aldrich Chemical, Milwaukee, Wis., 0.815 g, 5 mmole) in hot ethanol (10 ml) was mixed with a solution of dimethylaminoacethydrazide hydrochloride (Avocado/Alfa Aesar, Ward Hill, Mass.) in warm water (10 ml). The mixture was heated to reflux briefly and allowed to cool. After 3 hrs the mixture was diluted with 20 ml isopropanol, causing a copious precipitate to form. The precipitate was filtered out and washed with isopropanol. Drying gave 2.065 g (95%) white crystalline solid, melting pt. 280-282° C. (dec.).

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux briefly
  3. temperatureto cool
  4. customto form
  5. filtrationThe precipitate was filtered out
  6. washwashed with isopropanol
  7. customDrying

Quellen und Nachweise

ORD-Eintrag
ord-a926b4e75ec540909aa883a299f9a16c
Quelldatensatz
uspto-grants-2004_02
Patentnummer
US06689777B2

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