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2-(Methylamino)ethanol → 2-(N-(2,6-dimethyl-4-pyridyl)-N-methylamino)ethanol

HRID 279578
ノート
印刷プレビュー

反応式

HRID 279578 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH3:9])[CH:3]=1.[CH3:10][NH:11][CH2:12][CH2:13][OH:14]>Cl.O>[CH3:8][C:6]1[CH:7]=[C:2]([N:11]([CH2:12][CH2:13][OH:14])[CH3:10])[CH:3]=[C:4]([CH3:9])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 80162-(Methylamino)ethanolHCID 5881754-Chloro-2,6-dimethylpyridine

生成物 1

HCID 226250732-(N-(2,6-dimethyl-4-pyridyl)-N-methylamino)ethanol収率 90%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 962Water溶媒

実験手順

A solution of 4-chloro-2,6-dimethylpyridine (849 mg, 6 mmol), (J. Het. Chem. 1990, 1841), in 2-(methylamino)ethanol (1.35 g, 18 mmol) and 3M ethereal hydrogen chloride (3 drops) was heated at 140° C. for 1 hour. The reaction mixture was allowed to cool and was diluted with water. The insolubles were removed by filtration and the aqueous filtrate was poured onto a suspension of magnesium sulphate (50 g) in ethyl acetate (100 ml). The insolubles were removed by filtration and the filtrate dried (MgSO4) and the solvent removed by evaporation. The solid residue was triturated with ether, collected by filtration and dried under vacuum at 50° C. to give 2-(N-(2,6-dimethyl-4-pyridyl)-N-methylamino)ethanol (960 mg, 90%).

後処理

  1. temperatureto cool
  2. customThe insolubles were removed by filtration
  3. additionthe aqueous filtrate was poured onto a suspension of magnesium sulphate (50 g) in ethyl acetate (100 ml)
  4. customThe insolubles were removed by filtration
  5. dry with materialthe filtrate dried (MgSO4)
  6. customthe solvent removed by evaporation
  7. customThe solid residue was triturated with ether
  8. filtrationcollected by filtration
  9. customdried under vacuum at 50° C.

出典と根拠

ORDレコード
ord-2d5492c33cb443c0b6e913bd80d41aa9
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06362336B1

反応ノート

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