Hydrochloric Acid → HCID 19874067、化合物

HRID 465323ノート

反応式

HRID 465323 の反応式
[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

参加物

5

反応物 4

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

生成物 1

HCID 19874067HCID 19874067、化合物収率 65.6%

反応条件

温度
190 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8b250d89be7b4438b9b750e1f591b0d8
出典データセット
uspto-grants-1992_10
特許番号
US05153198

反応ノート

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