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Sodium Sulfate → HCID 563266、化合物

HRID 850458
ノート
印刷プレビュー

反応式

HRID 850458 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:7]([O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][C:22]#[N:23])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH2:7]([O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH2:21][CH2:22][NH2:23])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 5612222-BenzyloxyphenylacetonitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 563266HCID 563266、化合物収率 20.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

LAH (1.04 g, 0.0273 mol, 3.0 eq) was dissolved in THF (25 ml), and to this solution was added dropwise a THF solution (25 ml) of (2-benzyloxyphenyl)-acetonitrile (2.04 g, 0.0091 mol, 1.0 eq) under ice-cooling. After the completion of the dropwise addition, the mixture was stirred at room temperature for 15 minutes and refluxed under heating for 2 hours. This reaction mixture was cooled with ice-cold water, and a saturated aqueous sodium sulfate solution (about 30-40 ml) was added. After filtration through Celite, the filtrate was concentrated under reduced pressure. The obtained residue was purified by column chromatography (chloroforn/methanol=5/1) to give 2-(2-benzyloxyphenyl)ethylamine (0.415 g, 20.0%) as a pale-yellow amorphous compound.

後処理

  1. temperaturecooling
  2. additionAfter the completion of the dropwise addition
  3. temperaturerefluxed
  4. temperatureunder heating for 2 hours
  5. temperatureThis reaction mixture was cooled with ice-cold water
  6. filtrationAfter filtration through Celite
  7. concentrationthe filtrate was concentrated under reduced pressure
  8. customThe obtained residue was purified by column chromatography (chloroforn/methanol=5/1)

出典と根拠

ORDレコード
ord-c56bc94ff2694cb0891615538ed13200
出典データセット
uspto-grants-2000_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06017919

反応ノート

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