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Potassium Iodide → HCID 19874550, 화합물

HRID 465455
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HRID 465455 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 2733712Pyrazolidin-3-one hydrochlorideHCID 19874510HCID 19874510, 화합물

생성물 1

HCID 19874550HCID 19874550, 화합물

시약·촉매·용매 1

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

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bcf9f90175924dc1bdf3931b33b96a7d
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05153210

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