Hydrofluoric Acid → 7,8-Dichloro-3,4-dihydro-2H-1-benzopyran-4-one

반응식

[Cl:1][C:2]1[C:13]([Cl:14])=[CH:12][CH:11]=[CH:10][C:3]=1[O:4][CH2:5][CH2:6][C:7]([OH:9])=O.F>>[Cl:14][C:13]1[C:2]([Cl:1])=[C:3]2[C:10]([C:7](=[O:9])[CH2:6][CH2:5][O:4]2)=[CH:11][CH:12]=1

참가 물질

반응물 2

HCID 14917Hydrofluoric Acid

HCID 209930093-(2,3-Dichlorophenoxy)propanoic acid

생성물 1

HCID 126644077,8-Dichloro-3,4-dihydro-2H-1-benzopyran-4-one

실험 절차

500 mg of 3-(2,3-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

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

출처 및 근거

ORD 기록: ord-f483e257ffb744d194f075ebab8dcded
출처 데이터셋: uspto-grants-2015_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08969573B2

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