Tetrahydrofuran → 4-Bromo-7-isoquinolinamine

HRID 1173118ノート

反応式

HRID 1173118 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.O1CCCC1.[Cl-].[NH4+].[OH-].[Na+]>C(O)C.[Fe].O>[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 4

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 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 3

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

反応条件

温度
50 °C

実験手順

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

後処理

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe resulting residue was crystallized from isopropyl ether

出典と根拠

ORDレコード
ord-55d99ed0bf664372b1486baab47e5983
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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