Acetic Acid → HCID 69234598、化合物

HRID 1513627ノート

反応式

HRID 1513627 の反応式
[Br-:1].[CH2:2]([N+:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=O.[C:17]([O-])(=O)[CH3:18].[NH4+].[C:22]1(C)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.O.[C:30](O)(=O)[CH3:31]>>[Br:1][C:8]1[CH:7]=[CH:6][C:5]([C:3]2[C:2]([C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=3)=[N:11][C:16]([C:15]3[CH:14]=[CH:13][CH:12]=[CH:18][CH:17]=3)=[CH:30][CH:31]=2)=[CH:10][CH:9]=1

参加物

6

反応物 5

HCID 176Acetic AcidHCID 962WaterHCID 1140TolueneHCID 517165Ammonium AcetateHCID 27989541-(2-Oxo-2-phenylethyl)pyridin-1-ium bromide

生成物 1

HCID 69234598HCID 69234598、化合物収率 88%

実験手順

The synthetic intermediate (enone) 9.0 g 31 mmol), 1-phenacylpyridinium bromide 8.7 g (31 mmol) and ammonium acetate 19.3 g (25 mmol) were suspended in 27 ml of acetic acid and refluxed for 12 hours by heating. The reaction solution was cooled down to room temperature, and toluene and water were added thereto to separate the solution into two layers. Then, the organic layer was washed in order with a 10% sodium hydroxide aqueous solution and a saturated saline solution and dried on anhydrous sodium sulfate. After removing the organic solvent by distillation under reduced pressure, 27 ml of ethanol was added thereto, and deposited crystal was filtered and washed with ethanol to obtain 10.6 g (yield: 88%) of 4-bromophenyl-2,6-diphenylpyridine.

後処理

  1. temperaturerefluxed for 12 hours
  2. temperatureby heating
  3. customto separate the solution into two layers
  4. washThen, the organic layer was washed in order with a 10% sodium hydroxide aqueous solution
  5. dry with materiala saturated saline solution and dried on anhydrous sodium sulfate
  6. customAfter removing the organic solvent
  7. distillationby distillation under reduced pressure, 27 ml of ethanol
  8. additionwas added
  9. filtrationwas filtered
  10. washwashed with ethanol

出典と根拠

ORDレコード
ord-4da5c3006e9847cc8aa424e4ad337873
出典データセット
uspto-grants-2012_07
特許番号
US08217570B2

反応ノート

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