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Sodium Sulfite → HCID 178440164, 화합물

HRID 452183
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HRID 452183 반응식
[I:1][C:2]1[N:3]=[C:4]([CH2:8][CH2:9][CH3:10])[NH:5][C:6]=1I.S([O-])([O-])=O.[Na+].[Na+]>C(O)C.O>[I:1][C:2]1[N:3]=[C:4]([CH2:8][CH2:9][CH3:10])[NH:5][CH:6]=1
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참가 물질

4

반응물 2

HCID 24437Sodium SulfiteHCID 667341974,5-diiodo-2-propyl-1H-imidazole

생성물 1

HCID 178440164HCID 178440164, 화합물수율 88.2%

시약·촉매·용매 1

HCID 19096565Water ethanol용매

실험 절차

[step 1] 2-Propylimidazole (3.0 g, 27.3 mmol) was dissolved in dioxane/water (55 mL/55 mL), sodium hydrogen carbonate (8.67 g, 81.8 mmol) and iodine (15.0 g, 59.9 mmol) were added, and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture and the mixture was extracted 3 times with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 4,5-diiodo-2-propylimidazole (7.09 g, 72%). [step 2] 4,5-Diiodo-2-propylimidazole (3.0 g, 8.31 mmol) obtained in Reference Example A16, step 1 was dissolved in ethanol/water (60 mL/60 mL), sodium sulfite (8.40 g, 66.5 mmol) was added, and the mixture was heated under reflux overnight. After completion of the reaction, the mixture was extracted 3 times with chloroform. The combined organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 4-iodo-2-propylimidazole (1.73 g, 88%).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux overnight
  3. customAfter completion of the reaction
  4. extractionthe mixture was extracted 3 times with chloroform
  5. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e5e2d165fc6040568d0d934f0976cf1e
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486980B2

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