Water → 4-(Pyridin-4-yl)butan-1-amine

HRID 1719998ノート

反応式

HRID 1719998 の反応式
[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][CH2:9][C:10]#[N:11])=[CH:3][CH:2]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[N:1]1[CH:6]=[CH:5][C:4]([CH2:7][CH2:8][CH2:9][CH2:10][NH2:11])=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 135575314-(Pyridin-4-YL)butanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 135575324-(Pyridin-4-yl)butan-1-amine収率 6.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
10 °C

実験手順

The title product of Example 22(5.0 g, 34.0 mmol) in 40 mL of tetrahydrofuran was added dropwise to a stirred suspension of lithium aluminum hydride (LiAlH4, 3.2 g, 85.0 mmol) in 100 mL of THF over 20 minutes. The reaction was brought to reflux for 2 hours, cooled to 10° C., and treated with water (33.2 mL), 15% NaOH (3.2 mL), and then water (9.6 mL) again. The mixture was filtered and the solid was washed with Et2O. The filtrate was dried (Na2SO4), filtered, and stripped of solvent to yield 4.0 g of crude product that was distilled to produce the title compound (340 mg).

後処理

  1. temperatureto reflux for 2 hours
  2. filtrationThe mixture was filtered
  3. washthe solid was washed with Et2O
  4. dry with materialThe filtrate was dried (Na2SO4)
  5. filtrationfiltered
  6. customto yield 4.0 g of crude product that
  7. distillationwas distilled

出典と根拠

ORDレコード
ord-087111dc711f4f2c9f03488b123f389f
出典データセット
uspto-grants-1996_04
特許番号
US05504077

反応ノート

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