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2-(Methylamino)ethanol → 2-(N-(3,6-dichloropyridazin-4-yl)-N-methylamino)ethanol

HRID 279647
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HRID 279647 반응식
Br[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[N:4][C:3]=1[Cl:9].[CH3:10][NH:11][CH2:12][CH2:13][OH:14]>C(O)(C)C>[Cl:9][C:3]1[N:4]=[N:5][C:6]([Cl:8])=[CH:7][C:2]=1[N:11]([CH2:12][CH2:13][OH:14])[CH3:10]
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참가 물질

4

반응물 2

HCID 80162-(Methylamino)ethanolHCID 220306484-Bromo-3,6-dichloropyridazine

생성물 1

HCID 220307752-(N-(3,6-dichloropyridazin-4-yl)-N-methylamino)ethanol수율 90.1%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A solution of 4-bromo-3,6-dichloro-pyridazine (1.11 g, 5 mmol), (J.Chem. Soc., Perkin Trans I, 1974, 696), and 2-(methylamino)ethanol (0.75 g, 10 mmol) in isopropanol (10 ml) was heated at reflux for 30 minutes. The solvent was removed by evaporation, the residue was partitioned between methylene chloride and water and the aqueous layer was adjusted to pH9 with solid potassium carbonate. The organic layer was separated, washed with brine, dried (MgSO4) and the solvent removed by evaporation. The residue was triturated with ether, collected by filtration and dried under vacuum to give 2-(N-(3,6-dichloropyridazin-4-yl)-N-methylamino)ethanol (1 g, 90%).

후처리

  1. temperatureat reflux for 30 minutes
  2. customThe solvent was removed by evaporation
  3. customthe residue was partitioned between methylene chloride and water
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent removed by evaporation
  8. customThe residue was triturated with ether
  9. filtrationcollected by filtration
  10. customdried under vacuum

출처 및 근거

ORD 기록
ord-4f904d6a70204cd29e96137e805b5d12
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06362336B1

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