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2-(Methylamino)ethanol → (Z)-4-(1-(6-(2-(methylamino)ethoxy)pyridin-3-yl)-2-phenylbut-1-enyl)phenol

HRID 626096
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HRID 626096 반응식
[CH3:1][NH:2][CH2:3][CH2:4][OH:5].[H-].[Na+].Cl[C:9]1[N:14]=[CH:13][C:12](/[C:15](/[C:25]2[CH:30]=[CH:29][C:28]([OH:31])=[CH:27][CH:26]=2)=[C:16](\[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[CH2:17][CH3:18])=[CH:11][CH:10]=1>C1COCC1>[CH3:1][NH:2][CH2:3][CH2:4][O:5][C:9]1[N:14]=[CH:13][C:12](/[C:15](/[C:25]2[CH:26]=[CH:27][C:28]([OH:31])=[CH:29][CH:30]=2)=[C:16](\[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)/[CH2:17][CH3:18])=[CH:11][CH:10]=1
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참가 물질

5

반응물 3

HCID 80162-(Methylamino)ethanolHCID 24758Sodium hydrideHCID 71617026(Z)-4-(1-(6-chloropyridin-3-yl)-2-phenylbut-1-enyl)phenol

생성물 1

HCID 71617032(Z)-4-(1-(6-(2-(methylamino)ethoxy)pyridin-3-yl)-2-phenylbut-1-enyl)phenol수율 60%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 2-(methylamino)ethanol (672 mg, 10 eq) in 20 mL anhydrous THF was added NaH (373 mg, 8.0 eq) at 0° C. The mixture was stirred at rt for 1 h, then to the mixture was added (Z)-4-(1-(6-chloropyridin-3-yl)-2-phenylbut-1-enyl)phenol (300 mg, 1 eq, made from example 1). The reaction was heated at reflux for 16 h, cooled, quenched with sat. NH4Cl, and extracted with CH2Cl2. The extract was dried, concentrated, and purified by column chromatography to give the desired product (200 mg, 60% yield). 1H NMR (400 MHz, CDCl3) δ 7.59 (s, 1H), 7.18-7.20 (m, 2H), 7.08-7.16 (m, 3H), 7.01-7.06 (m, 3H), 6.77 (d, J=8.4 Hz, 1H), 6.28 (d, J=8.4 Hz, 1H), 4.28 (t, J=5.2 Hz, 2H), 2.93 (t, J=5.2 Hz, 2H), 2.46-2.55 (m, 5H), 0.92 (t, J=7.6 Hz, 3H); m/z=375 [M+1]+.

후처리

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 16 h
  3. temperaturecooled
  4. customquenched with sat. NH4Cl
  5. extractionextracted with CH2Cl2
  6. customThe extract was dried
  7. concentrationconcentrated
  8. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-f575dfa403134b59ac92a05d15068964
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09309211B2

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