Potassium Carbonate → 4-(tert-butyl)-N-[3-(2-hydroxyethoxy)-1-methyl-4-phenyl-1H-pyrazol-5-yl]-N-[(2-methoxyethoxy)methyl]benzenesulfonamide

HRID 1062787ノート

反応式

HRID 1062787 の反応式
C([O:4][CH2:5][CH2:6][O:7][C:8]1[C:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:11]([N:19]([S:26]([C:29]2[CH:34]=[CH:33][C:32]([C:35]([CH3:38])([CH3:37])[CH3:36])=[CH:31][CH:30]=2)(=[O:28])=[O:27])[CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])[N:10]([CH3:39])[N:9]=1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO.O>[C:35]([C:32]1[CH:33]=[CH:34][C:29]([S:26]([N:19]([C:11]2[N:10]([CH3:39])[N:9]=[C:8]([O:7][CH2:6][CH2:5][OH:4])[C:12]=2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])(=[O:28])=[O:27])=[CH:30][CH:31]=1)([CH3:38])([CH3:36])[CH3:37]

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 222820392-[(5-{{[4-(tert-butyl)phenyl]sulfonyl}[(2-methoxyethoxy)methyl]amino}-1-methyl-4-phenyl-1H-pyrazol-3-yl)oxy]ethyl acetate

生成物 1

HCID 222820064-(tert-butyl)-N-[3-(2-hydroxyethoxy)-1-methyl-4-phenyl-1H-pyrazol-5-yl]-N-[(2-methoxyethoxy)methyl]benzenesulfonamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To 2-[(5-{{[4-(tert-butyl)phenyl]sulfonyl}[(2-methoxyethoxy)methyl]amino}-1-methyl-4-phenyl-1H-pyrazol-3-yl)oxy]ethyl acetate (Preparation 16) (1.112 g) in solution in methanol (100 ml) was added a solution of potassium carbonate (890 mg) in water (25 ml), at room temperature. The reaction was stirred at room temperature for 1.5 hours, and then overnight. The reaction was stripped down and the residue partitioned between dichloromethane (20 ml) and water (20 ml). The aqueous layer was extracted with dichloromethane (10 ml). The organics were combined and back-washed with brine (10 ml). The solution was dried on magnesium sulfate, filtered and concentrated under reduced pressure to yield the desired product as an off white solid (528 mg)

後処理

  1. customat room temperature
  2. customovernight
  3. customthe residue partitioned between dichloromethane (20 ml) and water (20 ml)
  4. extractionThe aqueous layer was extracted with dichloromethane (10 ml)
  5. washback-washed with brine (10 ml)
  6. customThe solution was dried on magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1b70ceb665f141d99c5deadeea6ba89b
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…