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

HRID 454116
ノート
印刷プレビュー

反応式

HRID 454116 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-eaca31b71fe5436fb1cbd55ab81aa0d5
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492560B2

反応ノート

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