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

HRID 1420972
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HRID 1420972 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 962Water용매

실험 절차

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%).

후처리

  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.

출처 및 근거

ORD 기록
ord-b399511ab8b9468f841837e3418f5c07
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06071921

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