Acetone → HCID 14127187、化合物

HRID 1196991

反応式

HRID 1196991 の反応式
CC(C)=O.S([O-])([O-])(=O)=O.[Mg+2].P(O)([O-])([O-])=O.[Na+].[Na+].[Mn]([O-])(=O)(=O)=O.[Na+].[OH:24][CH:25]1[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[CH2:29][O:28][C:27]2[CH:36]=[CH:37][C:38]([CH2:40][CH2:41][O:42][C:43]([C:56]3[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=3)([C:50]3[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=3)[C:44]3[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=3)=[CH:39][C:26]1=2>CO.O>[O:24]=[C:25]1[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[CH2:29][O:28][C:27]2[CH:36]=[CH:37][C:38]([CH2:40][CH2:41][O:42][C:43]([C:56]3[CH:57]=[CH:58][CH:59]=[CH:60][CH:61]=3)([C:44]3[CH:45]=[CH:46][CH:47]=[CH:48][CH:49]=3)[C:50]3[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=3)=[CH:39][C:26]1=2

参加物

8

反応物 5

HCID 180AcetoneHCID 24083Sulfuric acid magnesium salt (1:1)HCID 24203Sodium Phosphate, DibasicHCID 15749399HCID 15749399、化合物HCID 23673458Sodium Permanganate

生成物 1

HCID 14127187HCID 14127187、化合物収率 80.3%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

In this process, 10 g of 11-hydroxy-2-(2-triphenylmethyloxyethyl)-6,11-dihydrodibenz[b,e]oxepin is dissolved in a solution comprising 800 ml of acetone, 1000 ml of water, 20 ml of saturated aqueous magnesium sulfate solution and 0.2 g of disodium phosphate. To the solution is dropwise added 2.6 g of aqueous sodium permanganate solution and the mixture is stirred at room temperature for 4.5 hours. Then, 100 ml of methanol is added thereto and the mixture is heated at reflux for 3 hours. After allowing the mixture to stand for cooling, the mixture is filtered and the filtrate is extracted with 1000 ml of ethyl acetate, washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is distilled away under reduced pressure and the resultant crude product is recrystallized from isopropanol to obtain 8.0 g of the desired product having melting point of 132-134° C. as a white crystal.

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 3 hours
  3. temperaturefor cooling
  4. filtrationthe mixture is filtered
  5. extractionthe filtrate is extracted with 1000 ml of ethyl acetate
  6. washwashed with saturated aqueous sodium chloride solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationThe solvent is distilled away under reduced pressure
  9. customthe resultant crude product is recrystallized from isopropanol

出典と根拠

ORDレコード
ord-9a9557da7f33423e9959bafa83096fa5
出典データセット
uspto-grants-1992_05
特許番号
US05116863

関連ノート

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