Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → 2-[3-(4-{[Benzyl(2-methyl-3-nitrophenyl)amino]methyl}phenoxy)phenoxy]ethanol

HRID 1370887노트

반응식

HRID 1370887 반응식
[CH2:1]([N:8]([C:33]1[CH:38]=[CH:37][CH:36]=[C:35]([N+:39]([O-:41])=[O:40])[C:34]=1[CH3:42])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([O:23][CH2:24][CH2:25][O:26]C3CCCCO3)[CH:18]=2)=[CH:12][CH:11]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>CCO.C(OCC)(=O)C>[CH2:1]([N:8]([CH2:9][C:10]1[CH:11]=[CH:12][C:13]([O:16][C:17]2[CH:18]=[C:19]([CH:20]=[CH:21][CH:22]=2)[O:23][CH2:24][CH2:25][OH:26])=[CH:14][CH:15]=1)[C:33]1[CH:38]=[CH:37][CH:36]=[C:35]([N+:39]([O-:41])=[O:40])[C:34]=1[CH3:42])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 18512355N-benzyl-N-(2-methyl-3-nitrophenyl)-N-(4-{3-[2-(tetrahydro-2H-pyran-2-yloxy)ethoxy]phenoxy}benzyl)amine

생성물 1

HCID 185122382-[3-(4-{[Benzyl(2-methyl-3-nitrophenyl)amino]methyl}phenoxy)phenoxy]ethanol

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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온도
55 °C

실험 절차

The product from Example 92A (0.480 g, 0.845 mmoles) in EtOH (2.0 mL) was treated with pyridinium p-toluenesulfonate (0.0106 g, 0.0422 mmoles) and heated at 55° C. for four hours. The reaction was diluted with ethyl acetate, washed with H2O, brine, dried (Na2SO4), filtered, and the filtrate concentrated under reduced pressure. The residue was purified by chromatography on a pre-packed Biotage silica gel column (hexanes to 50% ethyl acetate:hexanes) to provide the title compound.

후처리

  1. washwashed with H2O, brine
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under reduced pressure
  5. customThe residue was purified by chromatography on a pre-packed Biotage silica gel column (hexanes to 50% ethyl acetate:hexanes)

출처 및 근거

ORD 기록
ord-b3a80b3c5285430e8c5e6368e4c584b6
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06583180B2

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