N,N-Dimethylaniline → 2-Butyrylamino-4-methyl-3-nitropyridine

HRID 248368

反応式

HRID 248368 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1.CN(C)C1C=CC=CC=1.[C:21](Cl)(=[O:25])[CH2:22][CH2:23][CH3:24]>C(OCC)(=O)C>[C:21]([NH:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([CH3:11])[CH:5]=[CH:4][N:3]=1)(=[O:25])[CH2:22][CH2:23][CH3:24]

参加物

5

反応物 3

HCID 949N,N-DimethylanilineHCID 8855Butyryl chlorideHCID 2431662-Amino-4-methyl-3-nitropyridine

生成物 1

HCID 214642392-Butyrylamino-4-methyl-3-nitropyridine

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2-amino-4-methyl-3nitropyridine (5.0 g) and N,N-dimethylaniline (8.5 ml) was heated at 100° C. under nitrogen atmosphere. To the solution was added butyryl chloride (3.5 ml) and the mixture was stirred at 100° C. for 5 hours. After being cooled to room temperature, ethyl acetate was added to the reaction mixture. The organic layer was separated and washed successively with water and brine. The solution was dried over magnesium sulfate and the solvent was evaporated in vacuo. The residue was washed with n-hexane to give 2-butyrylamino-4-methyl-3-nitropyridine (7.0 g).

後処理

  1. temperatureAfter being cooled to room temperature
  2. customThe organic layer was separated
  3. washwashed successively with water and brine
  4. dry with materialThe solution was dried over magnesium sulfate
  5. customthe solvent was evaporated in vacuo
  6. washThe residue was washed with n-hexane

出典と根拠

ORDレコード
ord-9777e84daa0943d1869c526e16dd47ee
出典データセット
uspto-grants-1993_05
特許番号
US05210092

関連ノート

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