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

HRID 1370887ノート

反応式

HRID 1370887 の反応式
[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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
55 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b3a80b3c5285430e8c5e6368e4c584b6
出典データセット
uspto-grants-2003_06
特許番号
US06583180B2

反応ノート

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