Ammonia → 2-Isopropyl-5-nitropyridine

HRID 401411

반응식

HRID 401411 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 450963212-Isopropyl-5-nitropyridine수율 28.3%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
70 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c54b587836da45ddaf467f7055924490
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741925B2

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