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Ethanol → HCID 12399250, 화합물

HRID 1284087
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HRID 1284087 반응식
Cl[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:7][CH:6]=1)=O.C(O)C.[NH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][N:22]=1>CCOCC>[N:20]1[C:3]([C:5]2[CH:10]=[CH:9][C:8]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:7][CH:6]=2)=[CH:2][N:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 104392-AminopyridineHCID 12399236HCID 12399236, 화합물

생성물 1

HCID 12399250HCID 12399250, 화합물수율 39.4%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 96 g of ethyl 4-(chloroacetyl)phenylacetate, 200 ml of ethanol and 64 g of 2-aminopyridine is heated under reflux for 2 hours. The ethanol is distilled off under reduced pressure, and water is added to the residue. The mixture is extracted with benzene, and the extract is washed with water, dried and concentrated to give a brown oil. To the oil is added ether, and the crystalline precipitate is filtered off and recrystallized from a mixture of benzene and petroleum ether to give 44 g of ethyl 4-(imidazo[1,2-a]pyridin-2-yl)phenylacetate as pale brown crystals melting at 92°-93°C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. distillationThe ethanol is distilled off under reduced pressure, and water
  4. additionis added to the residue
  5. extractionThe mixture is extracted with benzene
  6. washthe extract is washed with water
  7. customdried
  8. concentrationconcentrated
  9. customto give a brown oil
  10. filtrationthe crystalline precipitate is filtered off
  11. customrecrystallized from a mixture of benzene and petroleum ether

출처 및 근거

ORD 기록
ord-3b1ab6daee694e8c9cfe81bfd4f2d7db
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03978071

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