Aluminium lithium hydride → 3-(Aminomethyl)-N-(2,4-dimethoxybenzyl)pyridin-2-amine

HRID 1172294

反応式

HRID 1172294 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:4]=1[CH2:5][NH:6][C:7]1[C:12]([C:13]#[N:14])=[CH:11][CH:10]=[CH:9][N:8]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>>[CH3:1][O:2][C:3]1[CH:18]=[C:17]([O:19][CH3:20])[CH:16]=[CH:15][C:4]=1[CH2:5][NH:6][C:7]1[C:12]([CH2:13][NH2:14])=[CH:11][CH:10]=[CH:9][N:8]=1

参加物

3

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 222931752-(2,4-Dimethoxybenzylamino)nicotinonitrile

生成物 1

HCID 222931603-(Aminomethyl)-N-(2,4-dimethoxybenzyl)pyridin-2-amine

実験手順

A solution of 2-(2,4-Dimethoxybenzylamino)pyridine-3-carbonitrile (0.55 g, 2.04 mmol) and LiAlH4 (2.2 ml of 1N, 4.4 mmol) was stirred at RT until the reaction was judged complete by LCMS. The reaction was quenched with sat. aq. Na2CO3 and the layers were separated. The organic layer was dried (Na2SO4) and the solvents removed under reduced pressure giving the desired product which was used without further purification. LC/MS (10% to 99%): M/Z (M+H)+ (obs)=274; tR=0.28.

後処理

  1. customThe reaction was quenched with sat. aq. Na2CO3
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. customthe solvents removed under reduced pressure

出典と根拠

ORDレコード
ord-dff5d436576f492d92676e077592d302
出典データセット
uspto-grants-2010_11
特許番号
US07834000B2

関連ノート

読み込み中…