Diethyl Ether → 2,2-Dimethylhexan-1-amine

HRID 26008

反応式

HRID 26008 の反応式
[CH3:1][C:2]([CH3:9])([CH2:5][CH2:6][CH2:7][CH3:8])[C:3]#[N:4].CCOCC.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O>[CH3:1][C:2]([CH3:9])([CH2:5][CH2:6][CH2:7][CH3:8])[CH2:3][NH2:4]

参加物

6

反応物 4

HCID 3283Diethyl Ether2 回HCID 14798Sodium HydroxideHCID 35735622,2-DimethylhexanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 543253312,2-Dimethylhexan-1-amine

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A solution of 2,2-dimethylcapronitrile (10.0 g., 0.078 mole) in 100 ml. of ether is added slowly to a suspension of lithium aluminum hydride (6.0 g., 0.158 mole) in 200 ml. of ether while maintaining the reaction at 0°-5°. After stirring the reaction mixture for an additional 2 hr., at 0.5°, the mixture is hydrolyzed by sequentially adding 6.0 ml. of water, 6.0 ml. of 15% sodium hydroxide solution, and finally 18 ml. of water. The hydrolyzed mixture is stirred for an additional hour, filtered and the ether phase concentrated under reduced pressure. Distillation of residual material provides 2,2-dimethylhex-1-ylamine.

後処理

  1. customthe reaction at 0°-5°
  2. customat 0.5°
  3. additionby sequentially adding 6.0 ml
  4. stirringThe hydrolyzed mixture is stirred for an additional hour
  5. filtrationfiltered
  6. concentrationthe ether phase concentrated under reduced pressure
  7. distillationDistillation of residual material

出典と根拠

ORDレコード
ord-eeed12b3af744259bd76c2d7e4263f32
出典データセット
uspto-grants-1979_04
特許番号
US04147805

関連ノート

読み込み中…