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Ozone → (RS)-2-(2-oxoethyl)-5,6-difluoro-1-indanone

HRID 264441
ノート
印刷プレビュー

反応式

HRID 264441 の反応式
[O:1]=[O+][O-].[CH2:4]([CH:8]1[CH2:16][C:15]2[C:10](=[CH:11][C:12]([F:18])=[C:13]([F:17])[CH:14]=2)[C:9]1=[O:19])[CH:5]=CC>ClCCl.CO>[O:1]=[CH:5][CH2:4][CH:8]1[CH2:16][C:15]2[C:10](=[CH:11][C:12]([F:18])=[C:13]([F:17])[CH:14]=2)[C:9]1=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24823Ozone2 回HCID 54100932(RS)-2-(2-buten-1-yl)-5,6-difluoro-1-indanone

生成物 1

HCID 19036408(RS)-2-(2-oxoethyl)-5,6-difluoro-1-indanone収率 76%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

An ozone stream (2 g ozone/hour) was conducted for 40 minutes while stirring through a solution, cooled to -70°, of 5.3 g of (RS)-2-(2-buten-1-yl)-5,6-difluoro-1-indanone in 125 ml of anhydrous dichloromethane and 25 ml of anhydrous methanol. Subsequently, the mixture was flushed with oxygen for 5 minutes and with argon for 10 minutes. After the addition of 2.64 ml of dimethyl sulfide, the mixture was stirred at room temperature for 16 hours. The reaction mixture was evaporated in a vacuum, the residue was treated with 60 ml of dichoromethane and, after the addition of 10 ml of water and 10 ml of trifluoroacetic acid, stirred at room temperature for 2 hours. The mixture was subsequently poured into 80 ml of water and neutralized by the spatula-wise addition of sodium hydrogen carbonate while stirring. An additional 40 ml of water were added, the phases were separated and the aqueous phase was extracted twice with 100 ml of dichloromethane each time. The combined organic phases were dried over magnesium sulfate and concentrated in a vacuum. There was obtained a yellow oil which was crystallized from diethyl ether/hexane. 3.82 g (76%) of (RS)-2-(2-oxoethyl)-5,6-difluoro-1-indanone were obtained as a white solid with m.p. 78°-81°.

後処理

  1. customSubsequently, the mixture was flushed with oxygen for 5 minutes and with argon for 10 minutes
  2. additionAfter the addition of 2.64 ml of dimethyl sulfide
  3. stirringthe mixture was stirred at room temperature for 16 hours
  4. customThe reaction mixture was evaporated in a vacuum
  5. additionthe residue was treated with 60 ml of dichoromethane
  6. additionafter the addition of 10 ml of water and 10 ml of trifluoroacetic acid
  7. stirringstirred at room temperature for 2 hours
  8. additionThe mixture was subsequently poured into 80 ml of water
  9. additionneutralized by the spatula-wise addition of sodium hydrogen carbonate
  10. stirringwhile stirring
  11. additionAn additional 40 ml of water were added
  12. customthe phases were separated
  13. extractionthe aqueous phase was extracted twice with 100 ml of dichloromethane each time
  14. dry with materialThe combined organic phases were dried over magnesium sulfate
  15. concentrationconcentrated in a vacuum
  16. customThere was obtained a yellow oil which
  17. customwas crystallized from diethyl ether/hexane

出典と根拠

ORDレコード
ord-6bed122bb3864127a7ad2dea0819cdfc
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05646173

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