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Water → (1-Ethylpiperidin-4-yl)methanamine

HRID 1790503
ノート
印刷プレビュー

反応式

HRID 1790503 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([N:10]1[CH2:15][CH2:14][CH:13]([CH2:16][NH2:17])[CH2:12][CH2:11]1)(=O)[CH3:8].O.[OH-].[Na+]>O1CCCC1.C(OCC)(=O)C>[CH2:7]([N:10]1[CH2:15][CH2:14][CH:13]([CH2:16][NH2:17])[CH2:12][CH2:11]1)[CH3:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 126870221-(4-(Aminomethyl)piperidin-1-yl)ethan-1-oneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 2794704(1-Ethylpiperidin-4-yl)methanamine収率 83.6%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

Lithium aluminum hydride (1.06 g) was suspended in tetrahydrofuran (70 ml) and the resultant suspension was stirred under nitrogen atmosphere under ice cooling. Next, 1-acetyl-4-aminomethylpiperidine (4.14 g). dissolved in tetrahydrofuran (30 ml) was added thereto and the resultant mixture was stirred at room temperature for 10 min and heated under reflux overnight. Then the reaction mixtures were ice-cooled and water (1.06 ml), a 5 N aqueous solution of sodium hydroxide (1.06 ml) and further water (3.18 ml) were successively added thereto. After stirring, the mixture was diluted with ethyl acetate and the insolubles were filtered off. The residue was purified by NH-silica gel column chromatography (chloroform/methanol system) to give the title compound (3.15 g) as a pale brown oil.

後処理

  1. additionwas added
  2. temperatureheated
  3. temperatureunder reflux overnight
  4. customThen the reaction mixtures
  5. temperaturecooled
  6. filtrationthe insolubles were filtered off
  7. customThe residue was purified by NH-silica gel column chromatography (chloroform/methanol system)

出典と根拠

ORDレコード
ord-73405c1cfbe74fcaa850e38e2982bcb1
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071201B2

反応ノート

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