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Ozone → (RS)-2-(2-oxoethyl)-6-ethyl-indanone

HRID 264420
ノート
印刷プレビュー

反応式

HRID 264420 の反応式
[O:1]=[O+][O-].[CH2:4]([CH:8]1[CH2:16][C:15]2[C:10](=[CH:11][C:12]([CH2:17][CH3:18])=[CH:13][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]([CH2:17][CH3:18])=[CH:13][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 54401231(RS)-2-(2-buten-1-yl)-6-ethyl-1-indanone

生成物 1

HCID 19036521(RS)-2-(2-oxoethyl)-6-ethyl-indanone収率 93%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

An ozone stream (3 g ozone/hour) was conducted for 40 minutes while stirring through a solution, cooled to -70°, of 7.92 g of (RS)-2-(2-buten-1-yl)-6-ethyl-1-indanone in 150 ml of anhydrous dichloromethane and 30 ml of anhydrous methanol. Subsequently, the mixture was flushed with oxygen for 5 minutes and with argon for 10 minutes. After the addition of 3.36 ml of dimethyl sulfide, the mixture was stirred at room temperature for 15 hours. The reaction mixture was evaporated in a vacuum. The residue was treated with 150 ml of dichoromethane and, after the addition of 30 ml of water and 30 ml of trifluoroacetic acid, stirred at room temperature for 3 hours. The mixture was subsequently poured into 150 ml of water and neutralized by the spatula-wise addition of sodium hydrogen carbonate while stirring. An additional 50 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. 6.94 g (93%) of (RS)-2-(2-oxoethyl)-6-ethyl-indanone were obtained as a yellow oil.

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 3.36 ml of dimethyl sulfide
  3. stirringthe mixture was stirred at room temperature for 15 hours
  4. customThe reaction mixture was evaporated in a vacuum
  5. additionThe residue was treated with 150 ml of dichoromethane
  6. additionafter the addition of 30 ml of water and 30 ml of trifluoroacetic acid
  7. stirringstirred at room temperature for 3 hours
  8. additionThe mixture was subsequently poured into 150 ml of water
  9. additionneutralized by the spatula-wise addition of sodium hydrogen carbonate
  10. stirringwhile stirring
  11. additionAn additional 50 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

出典と根拠

ORDレコード
ord-e6ddfb640df64e44b2e22e9dd33d01fc
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05646173

反応ノート

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