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2-[[(2-Methyl-4-nitrophenyl)sulfanyl]methyl]pyridine → 3-Methyl-4-[(2-pyridinylmethyl)sulfanyl]aniline

HRID 856682
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HRID 856682 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-])=O)[CH:5]=[CH:4][C:3]=1[S:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][C:3]=1[S:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1)[NH2:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 695222562-[[(2-Methyl-4-nitrophenyl)sulfanyl]methyl]pyridine

생성물 1

HCID 433032593-Methyl-4-[(2-pyridinylmethyl)sulfanyl]aniline수율 51%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To 2-[[(2-methyl-4-nitrophenyl)sulfanyl]methyl]pyridine (3.1 g) were added acetic acid (24.4 ml) and then, reduced iron (9.15 g), and the mixture was stirred for 16 hours at room temperature. The mixture was filtered with Celite, and washed with ethyl acetate. The solvent was removed under reduced pressure, and water was added to the obtained residue, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give 3-methyl-4-[(2-pyridinylmethyl)sulfanyl]aniline (1.4 g).

후처리

  1. filtrationThe mixture was filtered with Celite
  2. washwashed with ethyl acetate
  3. customThe solvent was removed under reduced pressure, and water
  4. additionwas added to the obtained residue
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was removed under reduced pressure
  9. customthe obtained residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2bd3ff3d49b14a4fb8daf34a33ec7000
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262185B2

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