Hydrochloric Acid → HCID 10198445, 화합물

HRID 231921노트

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HRID 231921 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]1(=[O:11])[O:10][C:8](=O)[CH2:7][CH2:6]1.C([O:15][C:16]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH:17]=1)(=O)C.Cl.[N+](C)([O-])=[O:26]>>[O:26]=[C:21]1[CH2:22][CH2:23][C:16](=[O:15])[CH:20]1[CH2:19][CH2:18][CH2:17][CH2:8][CH2:7][CH2:6][C:5]([OH:10])=[O:11]

참가 물질

6

실험 절차

To a solution of 2.7 g of aluminum chloride in 15 ml of nitromethane, 1.0 g of succinic anhydride was added, and then 1.7 g of 1-cyclooctenyl acetate was added dropwise under cooling. The resultant mixture was stirred at room temperature overnight and refluxed with stirring for four hours. The mixture was cooled, poured into 50 ml of 1N hydrochloric acid containing ice, and extracted four times with 30 ml of ethyl acetate. The organic layer was extracted twice with 30 ml of a saturated aqueous sodium bicarbonate solution. The aqueous layer was washed with ethyl acetate at pH 7. The aqueous was adjusted to pH 2 with 6N hydrochloric acid, and again extracted four times with 30 ml of ethyl acetate. The extract was dried and concentrated. The residue was washed with water to give 0.2 g of 7-(2,5-dioxocyclopentyl) heptanoic acid. This product had a melting point of 105° to 122° C.

후처리

  1. temperatureunder cooling
  2. temperaturerefluxed
  3. temperatureThe mixture was cooled
  4. additioncontaining ice
  5. extractionextracted four times with 30 ml of ethyl acetate
  6. extractionThe organic layer was extracted twice with 30 ml of a saturated aqueous sodium bicarbonate solution
  7. washThe aqueous layer was washed with ethyl acetate at pH 7
  8. extractionagain extracted four times with 30 ml of ethyl acetate
  9. customThe extract was dried
  10. concentrationconcentrated
  11. washThe residue was washed with water

출처 및 근거

ORD 기록
ord-bc84cc9f939f471da520bb265e00cb7e
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04849535

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