Hydrochloric Acid → HCID 19874067, 화합물

HRID 1534091노트

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HRID 1534091 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C([O-])=O.[NH4+:21].[ClH:22].[OH-].[Na+]>>[ClH:22].[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([NH2:21])[CH2:9][C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 2723923Ammonium formateHCID 27483631,2-Bis(4-fluorophenyl)ethanone

생성물 1

HCID 19874067HCID 19874067, 화합물수율 65.6%

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온도
190 °C

실험 절차

A mixture of 1,2-bis(4-fluorophenyl)-1-oxoethane (2.13 g) and ammonium formate (3.78 g) was stirred for 10 hours at 190° C.. After cooling, concentrated hydrochloric acid (12 ml) was added to the reaction mixture and the mixture was refluxed for 5 hours. After cooling, aqueous sodium hydroxide solution was added to the mixture and alkalized. The product was extracted with ethyl acetate and the organic layer was washed with saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo. The oily residue was dissolved in methanol. To the solution, HCl/methanol was added and the solution was concentrated in vacuo. Separated crystals were collected by filtration to give 1.77 g (65.6%) of the titled compound.

후처리

  1. temperatureAfter cooling
  2. temperaturethe mixture was refluxed for 5 hours
  3. temperatureAfter cooling
  4. extractionThe product was extracted with ethyl acetate
  5. washthe organic layer was washed with saturated sodium chloride solution
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. dissolutionThe oily residue was dissolved in methanol
  9. additionTo the solution, HCl/methanol was added
  10. concentrationthe solution was concentrated in vacuo
  11. customSeparated crystals
  12. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-36240fb79e9e4bd69f5e81dff48ac5a8
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05087627

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