Water → 2,5-Dibromo-3-nitropyridine

HRID 538572

反応式

HRID 538572 の反応式
[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

参加物

6

反応物 3

HCID 962WaterHCID 24614Phosphorus tribromideHCID 178418997HCID 178418997、化合物

生成物 1

HCID 2984702,5-Dibromo-3-nitropyridine収率 80.03%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-393084f0690840619769a6aea28260a2
出典データセット
uspto-grants-2014_10
特許番号
US08865736B2

関連ノート

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