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Iodine → HCID 12399250、化合物

HRID 1284094
ノート
印刷プレビュー

反応式

HRID 1284094 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 807IodineHCID 104392-AminopyridineHCID 73716Ethyl 4-acetylphenylacetate

生成物 1

HCID 12399250HCID 12399250、化合物収率 36.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e0166e7686ef44b18b89aaec796842ea
出典データセット
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03978071

反応ノート

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