Ammonia → 2-Isopropyl-5-nitropyridine

HRID 470116

反応式

HRID 470116 の反応式
C[N:2]1[CH:7]=[C:6]([N+]([O-])=O)[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[C:3]1=O.[CH3:15][CH:16](C)[C:17](=O)C.N>CO>[CH:16]([C:7]1[CH:6]=[CH:5][C:4]([N+:11]([O-:13])=[O:12])=[CH:3][N:2]=1)([CH3:17])[CH3:15]

参加物

5

反応物 3

HCID 222AmmoniaHCID 112513-Methyl-2-butanoneHCID 36212361-Methyl-3,5-dinitro-1H-pyridin-2-one

生成物 1

HCID 450963212-Isopropyl-5-nitropyridine収率 28.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
70 °C

実験手順

To a solution of 1-methyl-3,5-dinitro-2-pyridone (8.0 g, 40 mmol) in methyl alcohol (20 mL) was added dropwise 3-methyl-2-butanone (5.1 mL, 48 mmol), followed by ammonia solution in methyl alcohol (10.0 g, 17%, 100 mmol). The reaction mixture was heated at 70° C. for 2.5 h under atmospheric pressure. The solvent was removed under vacuum and the residual oil was dissolved in CH2Cl2, and then filtered. The filtrate was dried over Na2SO4 and concentrated to afford 2-isopropyl-5-nitro-pyridine (1.88 g, 28%).

後処理

  1. customThe solvent was removed under vacuum
  2. dissolutionthe residual oil was dissolved in CH2Cl2
  3. filtrationfiltered
  4. dry with materialThe filtrate was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-47d1cfcfb6b1412392cd0ff331ae130d
出典データセット
uspto-grants-2014_01
特許番号
US08629162B2

関連ノート

読み込み中…