Water → 4-Chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine

HRID 619730

반응식

HRID 619730 반응식
[Cl: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.O.[OH-].[Na+]>Cl>[Cl: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

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 218469034-Chloro-5-(5-isoquinolylsulfanyl)-2-nitroaniline

생성물 1

HCID 218469304-Chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine수율 89.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

4-Chloro-5-(5-isoquinolylsulfanyl)-2-nitroaniline 1.78 g (5.4 mmol) was dissolved in concentrated hydrochloric acid 30 ml, stannous chloride dihydrate 4.30 g (19.1 mmol) was added, and the mixture was stirred overnight at room temperature. The reaction mixture was poured into water, 50% sodium hydroxide was added to alkalize the mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and with saturated sodium chloride, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was recrystallized from ethyl acetate-n-hexane to give 4-chloro-5-(5-isoquinolylsulfanyl)-1,2-benzenediamine 1.45 g (89.5%).

후처리

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

출처 및 근거

ORD 기록
ord-064ef837141c4fd78d5569ce18e1284f
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05959107

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