6-Amino-3-chloropyridazine → 3-Amino-4-bromo-6-chloropyridazine

HRID 68445

반응식

HRID 68445 반응식
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.C([O-])(O)=O.[Na+].[Br:14]Br>CO>[Br:14][C:4]1[CH:3]=[C:2]([Cl:1])[N:7]=[N:6][C:5]=1[NH2:8]

참가 물질

5

반응물 3

HCID 216436-Amino-3-chloropyridazineHCID 24408BromineHCID 516892Sodium Bicarbonate

생성물 1

HCID 220244193-Amino-4-bromo-6-chloropyridazine수율 36%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 6-Chloro-pyridazin-3-ylamine (4 g, 31 mmol) in methanol (60 mL) was added NaHCO3 (5.2 g, 62 mmol). The reaction mixture was stirred for 30 minutes at RT then Br2 (4.9 g, 31 mmol) was added drop wise. Then the resulting reaction mixture was stirred additionally for 16 h at RT. After completion of reaction, the reaction mass concentrated under reduced pressure, crude purified by silica gel (100-200 mesh) chromatography using EtOAc/Hexane (8:2) to afford 4-Bromo-6-chloro-pyridazin-3-ylamine (2.3 g, 36%) as a solid.

후처리

  1. customThen the resulting reaction mixture
  2. stirringwas stirred additionally for 16 h at RT
  3. customAfter completion of reaction
  4. concentrationthe reaction mass concentrated under reduced pressure, crude
  5. custompurified by silica gel (100-200 mesh) chromatography

출처 및 근거

ORD 기록
ord-4e3baff1832d4fa7abb52f3c6518eb96
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822457B2

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