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7,8-Dichloro-3,4-dihydro-2H-1-benzopyran-4-one → HCID 67123949, 화합물

HRID 871055
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HRID 871055 반응식
[Cl:1][C:2]1[C:11]([Cl:12])=[C:10]2[C:5]([C:6](=[O:13])[CH2:7][CH2:8][O:9]2)=[CH:4][CH:3]=1.[Br-:14].[Br-].[Br-].[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1.[NH+]1C=CC=CC=1>C(O)C.C(Cl)(Cl)Cl>[Br:14][CH:7]1[C:6](=[O:13])[C:5]2[C:10](=[C:11]([Cl:12])[C:2]([Cl:1])=[CH:3][CH:4]=2)[O:9][CH2:8]1
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참가 물질

5

반응물 2

HCID 126644077,8-Dichloro-3,4-dihydro-2H-1-benzopyran-4-oneHCID 21124087Pyridiniumtribromide

생성물 1

HCID 67123949HCID 67123949, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6212Chloroform용매

실험 절차

A mixture of 100 mg. (0.46 mmol) 7,8-dichlorochroman-4-one was dissolved in anhydrous ethanol (5 ml) and Chloroform (5 ml). To this solution was added pyridinium tribromide (0.442 g, 1.38 mmol, 3 equiv). The reddish brown mixture was heated with stirring at 50 C for 30 min. The reaction mixture was then cooled and the solvent was evaporated. Then water (20 ml) was added to the residue and it was then extracted with 20 ml of dichloromethane. The dichloromethane layer was then washed with 5% sodium bicarbonate solution followed by water (20 ml). The organic layer was then dried and the solvent was evaporated in vacuum to yield the crude product which was purified by column chromatography.

후처리

  1. additionA mixture of 100 mg
  2. temperatureThe reddish brown mixture was heated
  3. temperatureThe reaction mixture was then cooled
  4. customthe solvent was evaporated
  5. additionThen water (20 ml) was added to the residue and it
  6. extractionwas then extracted with 20 ml of dichloromethane
  7. washThe dichloromethane layer was then washed with 5% sodium bicarbonate solution
  8. customThe organic layer was then dried
  9. customthe solvent was evaporated in vacuum

출처 및 근거

ORD 기록
ord-3a86c43775ef46b78a4810b047208f6c
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969573B2

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