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

HRID 581758노트

반응식

HRID 581758 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

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). mp: 134-135° C.

후처리

  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

출처 및 근거

ORD 기록
ord-36ab5f7774e6493bad4ff2ae16f7f5c9
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922711

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