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Water → (2-Aminomethyl-4-trifluoromethyl-phenyl)-cyclopropylmethyl-propyl-amine

HRID 604086
ノート
印刷プレビュー

反応式

HRID 604086 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:7]1([CH2:10][N:11]([CH2:25][CH2:26][CH3:27])[C:12]2[CH:20]=[CH:19][C:18]([C:21]([F:24])([F:23])[F:22])=[CH:17][C:13]=2[CH:14]=[N:15]O)[CH2:9][CH2:8]1.O.[OH-].[Na+]>O1CCCC1>[NH2:15][CH2:14][C:13]1[CH:17]=[C:18]([C:21]([F:23])([F:24])[F:22])[CH:19]=[CH:20][C:12]=1[N:11]([CH2:10][CH:7]1[CH2:9][CH2:8]1)[CH2:25][CH2:26][CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 866268392-(Cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime

生成物 1

HCID 43587121(2-Aminomethyl-4-trifluoromethyl-phenyl)-cyclopropylmethyl-propyl-amine

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

Lithium aluminum hydride (1.4 g) is suspended in tetrahydrofuran (50 ml) and thereto is added dropwise a 2-(cyclopropylmethyl-propyl-amino)-5-trifluoromethyl-benzaldehyde oxime (5.7 g) in tetrahydrofuran (20 ml) under ice-cooling, and the mixture is stirred at room temperature overnight. To the reaction solution are added water (1.4 ml), a 2N-aqueous sodium hydroxide solution (2.8 ml) and water (2.8 ml) successively under ice-cooling, and the insoluble material is removed by filtration and the filtrate is concentrated under reduced pressure. The resulting residue is purified by NH-silica gel column chromatography (chloroform:ethyl acetate=10:1) to give (2-aminomethyl-4-trifluoromethyl-phenyl)-cyclopropylmethyl-propyl-amine as a crude product (5.1 g).

後処理

  1. temperaturecooling
  2. customthe insoluble material is removed by filtration
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. customThe resulting residue is purified by NH-silica gel column chromatography (chloroform:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-4e33afa813bf404bba56c4b12bc2ec30
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07906517B2

反応ノート

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