Sodium Hydroxide → 4-Chloroisoquinolin-5-amine

HRID 10550

반응식

HRID 10550 반응식
O.O.[Sn](Cl)Cl.[Cl:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[N+:17]([O-])=O)[CH:10]=[N:9][CH:8]=1.[OH-].[Na+]>Cl>[Cl:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][C:15]=2[NH2:17])[CH:10]=[N:9][CH:8]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 219799674-Chloro-5-nitroisoquinoline

생성물 1

HCID 219799374-Chloroisoquinolin-5-amine수율 67.5%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

Tin(II) chloride dihydrate (1.70 g) was dissolved in concentrated hydrochloric acid (1 ml), added with a mixture of Intermediate 89 (315 mg) and 2 N aqueous hydrochloric acid (2 ml) with ice cooling and refluxed with heating for 2 hours. The reaction mixture was cooled to room temperature, added with 5 N aqueous sodium hydroxide (7 ml) and extracted twice with chloroform (20 ml for each time). The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain the title compound (182 mg).

후처리

  1. temperaturerefluxed
  2. temperaturewith heating for 2 hours
  3. extractionextracted twice with chloroform (20 ml for each time)
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-fcdc390576094c1d8a9ce9abd10a933f
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094789B2

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