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Dimethyl Sulfoxide → 2-Amino-5-fluoro-3-iodopyridine

HRID 78181
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HRID 78181 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][N:3]=1.CS(C)=O.[I:13]N1C(=O)CCC1=O.C(=O)([O-])O.[Na+]>C(O)(=O)C>[F:8][C:5]1[CH:6]=[C:7]([I:13])[C:2]([NH2:1])=[N:3][CH:4]=1
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참가 물질

6

반응물 4

HCID 679Dimethyl SulfoxideHCID 120273N-IodosuccinimideHCID 516892Sodium BicarbonateHCID 27377012-Amino-5-fluoropyridine

생성물 1

HCID 184559742-Amino-5-fluoro-3-iodopyridine수율 18%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a mixture of 2-amino-5-fluoropryidine (2.0 g, 17.8 mmol) and dimethyl sulfoxide (50 mL) was added N-iodosuccinimide (4.8 g, 21.4 mmol), which was stirred for 1 hour at room temperature. A suitable amount of acetic acid was added to this mixture, which was stirred for 1 hour at the same temperature, and then stirred for another 3 hours at 55° C. This reaction mixture was cooled to room temperature, after which a saturated sodium hydrogencarbonate aqueous solution was added, and the mixture was extracted with ethyl acetate. The organic layer was separated, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue thus obtained was purified by NH silica gel column chromatography (ethyl acetate) to obtain the title compound (751 mg, 18%).

후처리

  1. stirringwas stirred for 1 hour at the same temperature
  2. stirringstirred for another 3 hours at 55° C
  3. temperatureThis reaction mixture was cooled to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe organic layer was separated
  6. washwashed with water and saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated under a reduced pressure
  10. customthe residue thus obtained
  11. customwas purified by NH silica gel column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-004c2271435d4025ac26d2a86bf01c27
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841327B2

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