Tetrahydrofuran → 6-(Methylamino)-2-pyridylethanol

HRID 2416694ノート

反応式

HRID 2416694 の反応式
[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

参加物

4

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 21226445Aluminium lithium hydrideHCID 22507068Ethyl 2-(6-(methylamino)pyridin-2-yl)acetate

生成物 1

HCID 223194656-(Methylamino)-2-pyridylethanol

反応条件

温度
0 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-84fa2f6b76b74bac9bc50080b74a2d3d
出典データセット
uspto-grants-2004_11
特許番号
US06825188B2

反応ノート

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