Sodium Hydroxide → 4-Chloroisoquinolin-5-amine

HRID 10550

反応式

HRID 10550 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 219799374-Chloroisoquinolin-5-amine収率 67.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fcdc390576094c1d8a9ce9abd10a933f
出典データセット
uspto-grants-2006_08
特許番号
US07094789B2

関連ノート

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