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

HRID 248398

반응식

HRID 248398 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

A mixture of 2-amino-4-methyl-3-nitropyridine (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).

후처리

  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

출처 및 근거

ORD 기록
ord-9ce093bbe3ab4d4d9e23c434c5051e11
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210092

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