2-Chloropyridin-4-amine → 3-Bromo-2-chloropyridin-4-amine

HRID 219143

반응식

HRID 219143 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([Cl:8])[CH:3]=1.[Br:9]NC(=O)CCC(N)=O>C(O)(=O)C>[NH2:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([Cl:8])[C:3]=1[Br:9]

참가 물질

4

반응물 2

HCID 844322-Chloropyridin-4-amineHCID 9834204N-Bromosuccinamide

생성물 1

HCID 299193003-Bromo-2-chloropyridin-4-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4-amino-2-chloropyridine (50 g, 388 mmol) was dissolved in glacial acetic acid (500 mL). To this solution was added N-bromosuccinamide (75 g, 426 mmol,) portionwise at room temperature (water bath cooling was provided to control the exothermicity). The reaction mixture was stirred at RT for 1 h at which point the reaction was found complete (as monitored by TLC). Solvent was removed under reduced pressure followed by azeotropic distillation with ethanol. The crude product was purified by column chromatography on silica gel (230-400 mesh) eluting with ethyl acetate hexane mixture.

후처리

  1. temperaturecooling
  2. customwas provided
  3. customSolvent was removed under reduced pressure
  4. distillationfollowed by azeotropic distillation with ethanol
  5. customThe crude product was purified by column chromatography on silica gel (230-400 mesh)
  6. washeluting with ethyl acetate hexane mixture

출처 및 근거

ORD 기록
ord-f49c884ff4b54645b8e49b4da4d9151a
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198448B2

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