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Iodine → HCID 12399250, 화합물

HRID 1284094
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HRID 1284094 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:6][CH:5]=1)(=O)[CH3:2].II.[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][N:20]=1>C(O)C>[N:18]1[C:1]([C:4]2[CH:9]=[CH:8][C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:6][CH:5]=2)=[CH:2][N:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 807IodineHCID 104392-AminopyridineHCID 73716Ethyl 4-acetylphenylacetate

생성물 1

HCID 12399250HCID 12399250, 화합물수율 36.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 6 g of ethyl 4-acetylphenylacetate, 20 ml of ethanol, 7.5 g of iodine and 5.7 g of 2-aminopyridine is heated under reflux for 3 hours. The ethanol is distilled off under reduced pressure, and the residue is extracted with ethyl acetate. The extract is washed with water, dried, and concentrated to give a reddish brown oil. The oil is column chromatographed over silica gel with chloroform as eluent, and the colorless crystals obtained from the chloroform eluate are recrystallized from a mixture of benzene and petroleum ether to give 3.0 g of ethyl 4-(imidazo[1,2-a]pyridin-2-yl)phenylacetate melting at 92°-93°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 3 hours
  3. distillationThe ethanol is distilled off under reduced pressure
  4. extractionthe residue is extracted with ethyl acetate
  5. washThe extract is washed with water
  6. customdried
  7. concentrationconcentrated
  8. customto give a reddish brown oil
  9. customchromatographed over silica gel with chloroform as eluent
  10. customthe colorless crystals obtained from the chloroform eluate
  11. customare recrystallized from a mixture of benzene and petroleum ether

출처 및 근거

ORD 기록
ord-e0166e7686ef44b18b89aaec796842ea
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03978071

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