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

HRID 871057노트

반응식

HRID 871057 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-744efed30757469a8349614f11740e36
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969573B2

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