Stannous Chloride → 2,5-Dibromopyridin-3-amine

HRID 538573

반응식

HRID 538573 반응식
[Br:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1.Cl[Sn]Cl>C(O)C>[Br:1][C:2]1[C:7]([NH2:8])=[CH:6][C:5]([Br:11])=[CH:4][N:3]=1

참가 물질

4

반응 조건

온도
80 °C

실험 절차

To the solution of 2,5-Dibromo-3-nitro-pyridine (10.30 g, 35.47 mmol) in the 100 ml of ethanol was added SnCl2 (24.0 g, 106.42 mmol) slowly. The reaction mixture was heated at 80° C. for 2 h. After the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure. Water (250 mL) was added, white solid separated out, then, basified the reaction mixture with NaOH Solution. To this added the 250 ml of ethyl acetate. Filtered it and washed the residue with ethyl acetate, layers are separated, dried (Na2SO4), filtered, concentrated to give the desired product (6.20 g, 67.39%).

후처리

  1. customAfter the completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness under reduced pressure
  2. additionWater (250 mL) was added
  3. customwhite solid separated out
  4. additionTo this added the 250 ml of ethyl acetate
  5. filtrationFiltered it
  6. washwashed the residue with ethyl acetate, layers
  7. customare separated
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c271af90fdd74c5d8dee0187082e140a
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865736B2

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