Sodium Hydroxide → 4-(tert-butyl)-N-[1-methyl-4-(4-methylphenyl)-3-(2-phenoxyethoxy)-1H-pyrazol-5-yl]benzenesulfonamide

HRID 1062714ノート

反応式

HRID 1062714 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([N:14](S(C2C=CC(C(C)(C)C)=CC=2)(=O)=O)[C:15]2[N:19]([CH3:20])[N:18]=[C:17]([O:21][CH2:22][CH2:23][O:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:16]=2[C:31]2[CH:36]=[CH:35][C:34]([CH3:37])=[CH:33][CH:32]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>C(O)C.O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([S:11]([NH:14][C:15]2[N:19]([CH3:20])[N:18]=[C:17]([O:21][CH2:22][CH2:23][O:24][C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:16]=2[C:31]2[CH:36]=[CH:35][C:34]([CH3:37])=[CH:33][CH:32]=2)(=[O:13])=[O:12])=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 222819394-(tert-butyl)-N-{[4-(tert-butyl)phenyl]sulfonyl)-N-[1-methyl-4-(4-methylphenyl)-3-(2-phenoxyethoxy)-1H-pyrazol-5-yl]benzenesulfonamide

生成物 1

HCID 222819144-(tert-butyl)-N-[1-methyl-4-(4-methylphenyl)-3-(2-phenoxyethoxy)-1H-pyrazol-5-yl]benzenesulfonamide

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To 4-(tert-butyl)-N-{[4-(tert-butyl)phenyl]sulfonyl}-N-[1-methyl-4-(4-methylphenyl)-3-(2-phenoxyethoxy)-1H-pyrazol-5-yl]benzenesulfonamide (Preparation 1) (80 mg) in ethanol (20 ml) at room temperature was added sodium hydroxide (2N, 2 ml) and the mixture was stirred for 16 hrs. The mixture was reduced in volume to 10 ml under reduced pressure, diluted with water (50 ml) and extracted with ethyl acetate (30 ml). The organic fraction was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica (10 g) eluted with dichloromethane:ether (7:1) to yield the title compound as a colourless glass-like solid (7 mg).

後処理

  1. extractionextracted with ethyl acetate (30 ml)
  2. dry with materialThe organic fraction was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica (10 g)
  6. washeluted with dichloromethane:ether (7:1)

出典と根拠

ORDレコード
ord-9c8425566ea24a23a195ab86c04548dd
出典データセット
uspto-grants-2005_11
特許番号
US06962923B2

反応ノート

読み込み中…