Hydrochloric Acid → Acetate

HRID 650889

反応式

HRID 650889 の反応式
[F:1][C:2]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[S-2].[Li+].[Li+].Cl.[C:21]([O:24]CC)(=[O:23])[CH3:22]>CS(C)=O>[C:21]([O-:24])(=[O:23])[CH3:22].[F:1][C:2]1[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:3]=1[C:4]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1)=[O:5]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 5228262,5-DifluorobenzophenoneHCID 10290727Dilithium Sulfide

生成物 2

HCID 175AcetateHCID 5228262,5-Difluorobenzophenone

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

20 g (91.6 mmol) of 2,5-difluorobenzophenone 1 (Fluka) was dissolved in 400 ml of DMSO. 7.0 g (150 mmol) of lithium sulfide (Fluka) was added under argon. After three hours at 120° C., the mixture was allowed to cool to room temperature. It was shaken with 200 ml of 2 M HCl aq. and 500 ml of ethyl acetate. The organic phase was washed twice with NaCl solution, dried over MgSO4, filtered, and concentrated. 24 g of crude product 2 was obtained as a reddish oil. TLC (n-heptanelethyl acetate 3:1) gave Rf=0.3 (starting material 1 Rf=0.4). C13H9FOS (232.28). MS (M+H)+=233.1.

後処理

  1. washThe organic phase was washed twice with NaCl solution
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. custom24 g of crude product 2 was obtained as a reddish oil

出典と根拠

ORDレコード
ord-886445d07dde43e198f2aab5dbae20e2
出典データセット
uspto-grants-2001_08
特許番号
US06277831B1

関連ノート

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