Sodium Hydroxide → 4-Fluoro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine

HRID 619728

反応式

HRID 619728 の反応式
[F:1][C:2]1[C:8]([S:9][C:10]2[CH:19]=[CH:18][CH:17]=[C:16]3[C:11]=2[CH:12]=[CH:13][N:14]=[CH:15]3)=[CH:7][C:5]([NH2:6])=[C:4]([N+:20]([O-])=O)[CH:3]=1.[OH-].[Na+]>Cl>[F:1][C:2]1[CH:3]=[C:4]([NH2:20])[C:5]([NH2:6])=[CH:7][C:8]=1[S:9][C:10]1[CH:19]=[CH:18][CH:17]=[C:16]2[C:11]=1[CH:12]=[CH:13][N:14]=[CH:15]2

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 218469024-Fluoro-5-(5-isoquinolylsulfanyl)-2-nitroaniline

生成物 1

HCID 218469084-Fluoro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine収率 69.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

4-Fluoro-5-(5-isoquinolylsulfanyl)-2-nitroaniline 1.60 g (5.1 mmol) was dissolved in concentrated hydrochloric acid 30 ml, stannous chloride dihydrate 4.10 g (18.2 mmol) was added, and the mixture was stirred for 2 hours at room temperature. After 50% sodium hydroxide was added, the resulting alkaline solution was extracted with ethyl acetate. The organic layer was washed with water and saturated sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was recrystallized from ethyl acetate-n-hexane to obtain 4-fluoro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine 1.00 g (69.1%).

後処理

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

出典と根拠

ORDレコード
ord-14812b6731cd4dd38003d72eb9372e25
出典データセット
uspto-grants-1999_09
特許番号
US05959107

関連ノート

読み込み中…