Potassium Carbonate → 2-Bromo-4-methyl-3-nitro-pyridine

HRID 59958

反応式

HRID 59958 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][NH:5][C:4](=O)[C:3]=1[N+:9]([O-:11])=[O:10].P(Br)(Br)([Br:14])=O.C(=O)([O-])[O-].[K+].[K+]>ClC(Cl)C>[Br:14][C:4]1[C:3]([N+:9]([O-:11])=[O:10])=[C:2]([CH3:1])[CH:7]=[CH:6][N:5]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 24613Phosphorus oxybromideHCID 3453702-Hydroxy-4-methyl-3-nitropyridine

生成物 1

HCID 199260892-Bromo-4-methyl-3-nitro-pyridine収率 71.8%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒2 回

実験手順

The 4-methyl-3-nitropyridin-2(1H)-one (110 g, 0.71 mol) was suspended in dichloroethane (1 L). The solution of phosphorus oxybromide (317 g, 1.1 mol) in dichloroethane (1 L) was added dropwise thereto at the ambient temperature. The reaction mixture was refluxed for 12 hours. The mixture was allowed to cool to room temperature, poured into ice water, and neutralized with potassium carbonate. The organic layer was separated, washed with water and brine, and dried over sodium sulfate. The solvent was evaporated to provide the title compound (yield 71.8%).

後処理

  1. customat the ambient temperature
  2. temperatureThe reaction mixture was refluxed for 12 hours
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-ebac018909a54f20af991c206b66b15b
出典データセット
uspto-grants-2016_09
特許番号
US09440968B2

関連ノート

読み込み中…