1-Methylpiperazine → 4-Chloro-2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-one

HRID 42704노트

반응식

HRID 42704 반응식
[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1Cl.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>O>[Cl:1][C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[N:15]1[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]1

참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 1204623(2H)-Pyridazinone, 4,5-dichloro-2-methyl-

생성물 1

HCID 170880204-Chloro-2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 4,5-dichloro-2-methylpyridazin-3(2H)-one [S.-F. Chen and R. P. Panzica, J. Org. Chem., 46, 2467-2473 (1981)] (8.95 g, 50 mmol) and 1-methylpiperazine (12.5 g, 125 mmol) in water (150 ml) was refluxed for 30 h. After cooling, about two thirds of the solvent was removed under reduced pressure and the mixture was adjusted to pH 7-8 by addition of aqueous NaHCO3. It was then extracted with dichloromethane (4×40 ml) and the combined extracts were washed with water, dried (Na2SO4) and evaporated. The crude product was purified by recrystallization from ethanol (95%).

후처리

  1. temperaturewas refluxed for 30 h
  2. temperatureAfter cooling, about two thirds of the solvent
  3. customwas removed under reduced pressure
  4. additionthe mixture was adjusted to pH 7-8 by addition of aqueous NaHCO3
  5. extractionIt was then extracted with dichloromethane (4×40 ml)
  6. washthe combined extracts were washed with water
  7. dry with materialdried (Na2SO4)
  8. customevaporated
  9. customThe crude product was purified by recrystallization from ethanol (95%)

출처 및 근거

ORD 기록
ord-ca1ad0af93bd4ccb9e9e69a7dbd1a515
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536210B2

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