Sodium Hydroxide → HCID 21846995、化合物

HRID 619717ノート

反応式

HRID 619717 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10]([C:13]2[CH:22]=[CH:21][CH:20]=[C:19]3[C:14]=2[CH:15]=[CH:16][N:17]=[CH:18]3)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-])=O.[OH-].[Na+]>Cl.O>[CH:18]1[C:19]2[C:14](=[C:13]([S:10]([C:7]3[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][CH:6]=3)(=[O:12])=[O:11])[CH:22]=[CH:21][CH:20]=2)[CH:15]=[CH:16][N:17]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 154356855-(4-Nitrophenylsulfonyl)isoquinoline

生成物 1

HCID 21846995HCID 21846995、化合物収率 76.5%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

5-(4-Nitrophenylsulfonyl)isoquinoline 160 mg (0.6 mmol) was dissolved in concentrated hydrochloric acid 170 ml, stannous chloride dihydrate 650 mg (2.9 mmol) was added, and the mixture was stirred overnight at room temperature. 4 N sodium hydroxide in water was added to the reaction solution, and the resulting alkaline solution was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was recrystallized from methanol to give 4-(5-isoquinolylsulfonyl)aniline 110 mg (76.5%).

後処理

  1. extractionthe resulting alkaline solution was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated sodium chloride
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-5925996de9cc46f8bfd78c01cde72ea5
出典データセット
uspto-grants-1999_09
特許番号
US05959107

反応ノート

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