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Tetrahydrofuran → HCID 69967939, 화합물

HRID 1108895
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HRID 1108895 반응식
[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]
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참가 물질

4

반응물 3

HCID 8028Tetrahydrofuran2회HCID 21226445Aluminium lithium hydrideHCID 54539135HCID 54539135, 화합물

생성물 1

HCID 69967939HCID 69967939, 화합물

반응 조건

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-(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 x) gave the title compound as a colorless oil: MS (ES) 167 (M+H)+.

후처리

  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

출처 및 근거

ORD 기록
ord-cf64bb4b23ae4bef9eef92fff0305ff4
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06069158

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