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(3-Methoxymethoxypyridin-2-yl)-(4-nitrophenyl)methanol → 2-(4-Aminobenzyl)-3-methoxymethoxypyridine

HRID 1387925
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HRID 1387925 반응식
[CH3:1][O:2][CH2:3][O:4][C:5]1[C:6]([CH:11]([C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[CH:15][CH:14]=2)O)=[N:7][CH:8]=[CH:9][CH:10]=1>C(O)C.[Pd]>[NH2:19][C:16]1[CH:15]=[CH:14][C:13]([CH2:11][C:6]2[C:5]([O:4][CH2:3][O:2][CH3:1])=[CH:10][CH:9]=[CH:8][N:7]=2)=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 18472436(3-Methoxymethoxypyridin-2-yl)-(4-nitrophenyl)methanol

생성물 1

HCID 184722062-(4-Aminobenzyl)-3-methoxymethoxypyridine수율 29.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A mixture of (3-methoxymethoxypyridin-2-yl)-(4-nitrophenyl)methanol (11.78 g) and 10% Pd—C (1.2 g) in ethanol (100 ml) was vigorously stirred under hydrogen atmosphere for 24 hours. The catalyst was filtered of, and the filtrate was concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/hexane=1:1→2:1) to give 2-(4-aminobenzyl)-3-methoxymethoxypyridine (2.92 g) as orange oil.

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후처리

  1. filtrationThe catalyst was filtered of, and the filtrate
  2. concentrationwas concentrated under reduced pressure
  3. customThe residue was separated
  4. custompurified with column chromatography (ethyl acetate/hexane=1:1→2:1)

출처 및 근거

ORD 기록
ord-00772021b89048caadb83c599d899276
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06268354B1

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