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

HRID 2120092노트

반응식

HRID 2120092 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-a926b4e75ec540909aa883a299f9a16c
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06689777B2

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