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Potassium Iodide → HCID 19874550、化合物

HRID 465455
ノート
印刷プレビュー

反応式

HRID 465455 の反応式
[CH2:1]([C:5]1[CH:22]=[CH:21][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]Br)=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3].C(=O)([O-])[O-].[K+].[K+].Cl.[NH:30]1[CH2:34][CH2:33][C:32](=[O:35])[NH:31]1.[I-].[K+]>C(#N)C.O>[CH2:1]([C:5]1[CH:22]=[CH:21][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:30]2[CH2:34][CH2:33][C:32](=[O:35])[NH:31]2)=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 2733712Pyrazolidin-3-one hydrochlorideHCID 19874510HCID 19874510、化合物

生成物 1

HCID 19874550HCID 19874550、化合物

試薬・触媒・溶媒 1

HCID 18373917Acetonitrile--water (1/1)溶媒

実験手順

A mixture of 10-(4-acetonylphenoxy)decylbromide, ethylene ketal (3.0 g), potassium carbonate (3.8 g), pyrazolidin-3-one hydrochloride (1.47 g) and potassium iodide (0.5 g) in acetonitrile:water (95:5), was heated under reflux for 3 hr. The reaction mixture was allowed to cool, filtered and the solvent evaporated in vacuo. The residue was dissolved in chloroform, washed with water (2×50 ml), dried (magnesium sulphate), fitered and the solvent removed in vacuo. The residue was dissolved in acetone (50 ml) and treated with 2M hydrochloric acid solution (3 ml) and allowed to stand at room temperature for 3 hr. The solvent was removed in vacuo and the residue was dissolved in chloroform and washed with 1.2M sodium bicarbonate solution (1×50 ml), water (2×50 ml), dried (magnesium sulphate), filtered and the solvent removed in vacuo to give 1-[10-(4-acetonylphenoxy)decyl]pyrazolidin-3-one (0.66 g).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hr
  3. temperatureto cool
  4. filtrationfiltered
  5. customthe solvent evaporated in vacuo
  6. dissolutionThe residue was dissolved in chloroform
  7. washwashed with water (2×50 ml)
  8. dry with materialdried (magnesium sulphate)
  9. customthe solvent removed in vacuo
  10. dissolutionThe residue was dissolved in acetone (50 ml)
  11. additiontreated with 2M hydrochloric acid solution (3 ml)
  12. customThe solvent was removed in vacuo
  13. dissolutionthe residue was dissolved in chloroform
  14. washwashed with 1.2M sodium bicarbonate solution (1×50 ml), water (2×50 ml)
  15. dry with materialdried (magnesium sulphate)
  16. filtrationfiltered
  17. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-bcf9f90175924dc1bdf3931b33b96a7d
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05153210

反応ノート

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