Bromine → 6-Bromo-2-fluoropyridin-3-amine

HRID 59938

반응식

HRID 59938 반응식
[F:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.CC([O-])=O.[K+].[Br:14]Br>CC(O)=O>[Br:14][C:4]1[N:3]=[C:2]([F:1])[C:7]([NH2:8])=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 24408BromineHCID 517044Potassium AcetateHCID 27628162-Fluoropyridin-3-amine

생성물 1

HCID 594247976-Bromo-2-fluoropyridin-3-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 2-fluoropyridin-3-amine (44.6 mmol) and KOAc (44.6 mmol) in AcOH was stirred at room temperature for 1 h. The mixture was cooled to 0 C and Br2 (44.6 mmol) was added dropwise. The mixture was stirred at 0° C. for 15 min. The mixture was concentrated and the residue was dissolved in EtOAc/MeOH. The organic solution was washed (sat. NaHCO3, sat. Na2S2O3), dried (Na2SO4) and concentrated. The residue was purified by flash column chromatography (SiO2, 100:0 to 80:20 petroleum ether/EtOAc) to yield the desired product.

후처리

  1. additionwas added dropwise
  2. stirringThe mixture was stirred at 0° C. for 15 min
  3. concentrationThe mixture was concentrated
  4. dissolutionthe residue was dissolved in EtOAc/MeOH
  5. washThe organic solution was washed (sat. NaHCO3, sat. Na2S2O3)
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated
  8. customThe residue was purified by flash column chromatography (SiO2, 100:0 to 80:20 petroleum ether/EtOAc)

출처 및 근거

ORD 기록
ord-ebefc4c650fd47febf3c6cbbab7a5010
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440929B2

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