Water → 2,5-Dibromo-3-nitropyridine

HRID 538572

반응식

HRID 538572 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](O)=[N:6][CH:7]=1.P(Br)(Br)[Br:13].O>C1(C)C=CC=CC=1.CN(C=O)C>[Br:13][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]([Br:1])=[CH:7][N:6]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 178418997HCID 178418997, 화합물

생성물 1

HCID 2984702,5-Dibromo-3-nitropyridine수율 80.03%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

반응 조건

온도
120 °C

실험 절차

To a solution of 5-Bromo-3-nitro-pyridin-2-ol (10.0 g, 45.66 mmol) in 70 ml of toluene and 7 ml of DMF was added PBr3 (6.60 ml, 68.49 mmol) and the reaction mixture was heated at 120° C. for 20 min under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (100 mL) was added and extracted with ethyl acetate (3×200 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated to get the desired product (10.30 g, 80.03%).

후처리

  1. extractionextracted with ethyl acetate (3×200 mL)
  2. washThe combined organics was washed with water, brine
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-393084f0690840619769a6aea28260a2
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865736B2

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