Sodium Chloride → 4-Bromo-7-isoquinolinamine

HRID 1005676노트

반응식

HRID 1005676 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.[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

참가 물질

8

반응물 3

HCID 5234Sodium ChlorideHCID 25517Ammonium ChlorideHCID 22674041HCID 22674041, 화합물

생성물 1

HCID 226740574-Bromo-7-isoquinolinamine수율 56.9%

시약·촉매·용매 4

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-857f900068b04f0ab88ac8ee3edf31cd
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787534B2

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