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

HRID 2120092ノート

反応式

HRID 2120092 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-a926b4e75ec540909aa883a299f9a16c
出典データセット
uspto-grants-2004_02
特許番号
US06689777B2

反応ノート

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