Hydrofluoric Acid → 6,7-Dichloro-2,3-dihydro-4H-1-benzopyran-4-one

HRID 871057ノート

反応式

HRID 871057 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[CH:12][C:13]=1[Cl:14])[O:5][CH2:6][CH2:7][C:8]([OH:10])=O.F>>[Cl:14][C:13]1[CH:12]=[C:11]2[C:4](=[CH:3][C:2]=1[Cl:1])[O:5][CH2:6][CH2:7][C:8]2=[O:10]

参加物

3

反応物 2

HCID 14917Hydrofluoric AcidHCID 8193113-(3,4-Dichlorophenoxy)propanoic acid

生成物 1

HCID 126644086,7-Dichloro-2,3-dihydro-4H-1-benzopyran-4-one

実験手順

500 mg of 3-(3,4-dichlorophenoxy)propionic acid, is stirred in 50 ml. of liquid hydrogen fluoride surrounded by a solid carbon dioxide/acetone bath. This slurry is allowed to stir overnight without replenishing the cooling bath. The hydrogen fluoride is removed by a stream of air. The residual solid was then dissolved in ether and washed with 10% aqueous sodium carbonate solution. The organic layer is dried over anhydrous magnesium sulphate and the solvent is evaporated to give the required chromanone with sufficient purity.

後処理

  1. customThe hydrogen fluoride is removed by a stream of air
  2. dissolutionThe residual solid was then dissolved in ether
  3. washwashed with 10% aqueous sodium carbonate solution
  4. dry with materialThe organic layer is dried over anhydrous magnesium sulphate
  5. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-744efed30757469a8349614f11740e36
出典データセット
uspto-grants-2015_03
特許番号
US08969573B2

反応ノート

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