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Tetrahydrofuran → HCID 69967939、化合物

HRID 636304
ノート
印刷プレビュー

反応式

HRID 636304 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH2:16][C:17](OCC)=O)[N:11]=1)[CH3:8].C1C[O:25]CC1>>[CH2:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([CH:16]([OH:25])[CH3:17])[N:11]=1)[CH3:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 21226445Aluminium lithium hydrideHCID 54539135HCID 54539135、化合物

生成物 1

HCID 69967939HCID 69967939、化合物

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-(ethylamino)-6-pyridylacetate (1 g, 4.1 mmol) in THF (30 mL). After the addition was completed, the reaction mixture was heated to reflux. After 5 hr, the reaction was cooled 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) 167 (M+H)+.

後処理

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

出典と根拠

ORDレコード
ord-ca20b08a430346f4bff2ecc280513b1a
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06191304B1

反応ノート

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