Potassium Carbonate → 3-Methyl-5-nitroisoquinoline

HRID 559477

반응식

HRID 559477 반응식
[CH3:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.[N+:12]([O-])([O-:14])=[O:13].[K+].C(=O)([O-])[O-].[K+].[K+]>S(=O)(=O)(O)O>[CH3:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([N+:12]([O-:14])=[O:13])[CH:8]=[CH:7][CH:6]=2

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 143063-MethylisoquinolineHCID 24434Potassium Nitrate

생성물 1

HCID 2749733-Methyl-5-nitroisoquinoline

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

A solution of 3-methylisoquinoline (5.4 g, 0.038 mol) in concentrated sulfuric acid (30 ml) was cautiously added to a solution of potassium nitrate (4.25 g, 1.1 eq) in concentrated sulfuric acid (23 ml) whilst maintaining the temperature below 4° C. (ice bath). Stirring was continued for 2 h and then temperature raised to ambient. Reaction was further stirred for 3 h and then poured into ice-water slurry (500 ml). Neutralisation using solid potassium carbonate afforded a yellow solid which was filtered and washed with water. The crude product was dissolved in ethanol (200 ml), filtered and concentrated under reduced pressure to afford the title compound as a yellow solid.

후처리

  1. temperaturewhilst maintaining the temperature below 4° C. (ice bath)
  2. temperaturetemperature raised to ambient
  3. customReaction
  4. stirringwas further stirred for 3 h
  5. customafforded a yellow solid which
  6. filtrationwas filtered
  7. washwashed with water
  8. dissolutionThe crude product was dissolved in ethanol (200 ml)
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-76441f1f554e4a10a36349439a94c7dd
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063078B2

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