Water → 2-Methyl-2-(morpholin-4-yl)propan-1-amine

HRID 264946ノート

反応式

HRID 264946 の反応式
[CH3:1][C:2]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)([CH3:6])[C:3]([NH2:5])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:5][CH2:3][C:2]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)([CH3:6])[CH3:1]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 74719562-Methyl-2-morpholin-4-ylpropanamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 19896412-Methyl-2-(morpholin-4-yl)propan-1-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 8.33 g of 2-methyl-2-morpholino-propionic acid amide in 50 ml of tetrahydrofuran is slowly added at room temperature to 3.33 g of lithium aluminium hydride in 85 ml of tetrahydrofuran. The reaction mixture is then stirred for a further 2 hours under reflux. The reaction mixture is cooled and then 5 ml of water, 6.67 ml of 2N sodium hydroxide and a further 5 ml of water are added in succession. The suspension is clarified by filtration and the crude title compound is obtained from the concentrated filtrate: 1H NMR (CDCl3), δ(ppm)=3.67 (4H, m), 2.52 (2H, s), 2.48 (4H, m), 1.37 (2H, bs),0.92 (6H, s).

後処理

  1. temperatureunder reflux
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe suspension is clarified by filtration

出典と根拠

ORDレコード
ord-ccb30767d6824311a4ed2e39c394adb5
出典データセット
uspto-grants-1997_07
特許番号
US05646143

反応ノート

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