Tetrahydrofuran → 6-(Methylamino)-2-pyridylethanol

HRID 2416694노트

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HRID 2416694 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].C(O[C:10](=O)[CH2:11][C:12]1[N:17]=[C:16]([NH:18][CH3:19])[CH:15]=[CH:14][CH:13]=1)C.C1C[O:24]CC1>>[CH3:19][NH:18][C:16]1[N:17]=[C:12]([CH:11]([OH:24])[CH3:10])[CH:13]=[CH:14][CH:15]=1

참가 물질

4

반응물 3

HCID 8028Tetrahydrofuran2회HCID 21226445Aluminium lithium hydrideHCID 22507068Ethyl 2-(6-(methylamino)pyridin-2-yl)acetate

생성물 1

HCID 223194656-(Methylamino)-2-pyridylethanol

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온도
0 °C

실험 절차

To a mechanically stirred solution of LiAlH4 in THF (1.0 M, 20 mL, 20.4 mmol) was added dropwise a solution of ethyl-2-(methylamino)-6-pyridylacetate (0.38 g, 2 mmol) in THF (10 mL). After the addition was completed, the reaction mixture was warmed to 0° C. and quenched with 10% NaOH solution. The solids were removed by filtration, and the filtrate was concentrated in vacuum. The residue was dissolved in CH2Cl2 and the solution was dried (MgSO4) and concentrated. Reconcentration from toluene (3×) gave the title compound as a colorless oil: MS (ES) m/e 153 (M+H)+.

후처리

  1. additionAfter the addition
  2. customquenched with 10% NaOH solution
  3. customThe solids were removed by filtration
  4. concentrationthe filtrate was concentrated in vacuum
  5. dissolutionThe residue was dissolved in CH2Cl2
  6. dry with materialthe solution was dried (MgSO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-84fa2f6b76b74bac9bc50080b74a2d3d
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825188B2

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