Tetrahydrofuran → 4-Bromo-7-isoquinolinamine

HRID 1173118노트

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HRID 1173118 반응식
[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

참가 물질

8

반응물 4

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 22674041HCID 22674041, 화합물

생성물 1

HCID 226740574-Bromo-7-isoquinolinamine수율 56.9%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-55d99ed0bf664372b1486baab47e5983
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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