Sodium Chloride → 4-Bromo-7-isoquinolinamine

HRID 1005676ノート

反応式

HRID 1005676 の反応式
[N+:1]([C:4]1[CH:13]=[C:12]2[C:7]([C:8]([Br:14])=[CH:9][N:10]=[CH:11]2)=[CH:6][CH:5]=1)([O-])=O.[Cl-].[NH4+].[Cl-].[Na+]>C(O)C.O1CCCC1.O.[Fe]>[NH2:1][C:4]1[CH:13]=[C:12]2[C:7]([C:8]([Br:14])=[CH:9][N:10]=[CH:11]2)=[CH:6][CH:5]=1

参加物

8

反応物 3

HCID 5234Sodium ChlorideHCID 25517Ammonium ChlorideHCID 22674041HCID 22674041、化合物

生成物 1

HCID 226740574-Bromo-7-isoquinolinamine収率 56.9%

試薬・触媒・溶媒 4

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 1 ml of ethanol, 2 ml of tetrahydrofuran and 1 ml of water was dissolved 66 mg (0.26 mmol) of 7-nitro-4-bromoisoquinoline, and 70 mg of powdered iron and 140 mg of ammonium chloride were added thereto, followed by heating at 50 degrees for 3 hours. To the reaction mixture was added 1 N sodium chloride aqueous solution, followed by extracting with chloroform. The organic layer was dried over magnesium sulfate and concentrated. Then, the resulting residue was crystallized from isopropyl ether, to give 33 mg of the title compound.

後処理

  1. additionwere added
  2. temperatureby heating at 50 degrees for 3 hours
  3. extractionby extracting with chloroform
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThen, the resulting residue was crystallized from isopropyl ether

出典と根拠

ORDレコード
ord-857f900068b04f0ab88ac8ee3edf31cd
出典データセット
uspto-grants-2004_09
特許番号
US06787534B2

反応ノート

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