benzyl N-(2-methoxyethyl)-N-(3-pyridylmethyl)carbamate → (2-Methoxyethyl)(pyridin-3-ylmethyl)amine

HRID 564915ノート

反応式

HRID 564915 の反応式
[CH3:1][O:2][CH2:3][CH2:4][N:5]([CH2:16][C:17]1[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=1)C(=O)OCC1C=CC=CC=1>[Pd].C(O)C>[CH3:1][O:2][CH2:3][CH2:4][NH:5][CH2:16][C:17]1[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=1

参加物

4

反応物 1

HCID 22112998benzyl N-(2-methoxyethyl)-N-(3-pyridylmethyl)carbamate

生成物 1

HCID 4720010(2-Methoxyethyl)(pyridin-3-ylmethyl)amine収率 43.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of benzyl N-(2-methoxyethyl)-N-(3-pyridylmethyl)carbamate (5.4 g) and 10% palladium on carbon (1.0 g) in ethanol (50 ml) was stirred under hydrogen atmosphere for 9 hours. The catalyst was removed by filtration, and the filtrate was concentrated under azeotropic condition with toluene and ethanol. The residue was dissolved in ethanol and diethyl ether was added thereto to give precipitates, which were collected by filtration to give N-(2-methoxyethyl)-N-(3-pyridylmethyl)amine (1.3 g).

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under azeotropic condition with toluene and ethanol
  3. dissolutionThe residue was dissolved in ethanol
  4. additiondiethyl ether was added
  5. customto give
  6. customprecipitates
  7. filtrationwhich were collected by filtration

出典と根拠

ORDレコード
ord-caebe7d3a6ff483899e5d695ae1a0e36
出典データセット
uspto-grants-2001_01
特許番号
US06169095A

反応ノート

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