Nitric Acid → 3-Ethoxy-2-methyl-6-nitropyridine

HRID 847769

반응식

HRID 847769 반응식
[CH2:1]([O:3][C:4]1[C:5]([CH3:10])=[N:6][CH:7]=[CH:8][CH:9]=1)[CH3:2].[N+:11]([O-])([OH:13])=[O:12]>S(=O)(=O)(O)O>[CH2:1]([O:3][C:4]1[C:5]([CH3:10])=[N:6][C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=1)[CH3:2]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 128750153-Ethoxy-2-methylpyridine2회

생성물 1

HCID 128750163-Ethoxy-2-methyl-6-nitropyridine

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

To a solution of 70 g of 3-ethoxy-2-methylpyridine (Compound II where R2 =C2H5) dissolved in 280 ml of sulfuric acid under ice-cooling, a mixed solution of 42 ml of fuming nitric acid and 50 ml of concentrated sulfuric acid was added dropwise while stirring and keeping the internal temperature at 0° to 3° C. After stirring for additional 30 minutes at the same temperature, the reaction mixture was poured into ice water and extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and concentrated to give 85 g of 3-ethoxy-2-methyl-6-nitropyridine (Compound III where R2 =C2H5), m.p. 90°-92° C.

후처리

  1. temperaturecooling
  2. customat 0° to 3° C
  3. stirringAfter stirring for additional 30 minutes at the same temperature
  4. extractionextracted with chloroform
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b74d1ccab8e94512af1236e7261d7542
출처 데이터셋
uspto-grants-1981_10
특허 번호
US04293695

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