Potassium Persulfate → 2,3-Dihydro-2,2-dimethyl-7-nitrobenzofuran-3-one

HRID 440660

반응식

HRID 440660 반응식
[CH3:1][C:2]1([CH3:14])[CH2:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:4]=2[O:3]1.S(OOS([O-])(=O)=O)([O-])(=O)=[O:16].[K+].[K+]>C(#N)C.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[CH3:1][C:2]1([CH3:14])[C:6](=[O:16])[C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:4]=2[O:3]1

참가 물질

6

반응물 2

HCID 24412Potassium PersulfateHCID 834162,3-Dihydro-2,2-dimethyl-7-nitrobenzofuran

생성물 1

HCID 224047252,3-Dihydro-2,2-dimethyl-7-nitrobenzofuran-3-one수율 93.5%

시약·촉매·용매 3

HCID 24463Copper sulfate pentahydrate촉매HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

A mixture of 37.3 g (0.193 mole) of 2,3-dihydro-2,2-dimethyl-7-nitrobenzofuran, 156.6 g (0.58 mole) of potassium persulfate, and 48.2 g (0.193 mole) of copper(II) sulfate pentahydrate in 500 mL of acetonitrile and 500 mL of water was prepared. This mixture was heated at reflux for one hour with vigorous stirring. The reaction mixture was cooled and then extracted three times with methylene chloride. The combined extracts were dried over anhydrous magnesium sulfate, filtered, and the solvent was evaporated from the filtrate under reduced pressure, leaving 37.4 g of 2,3-dihydro-2,2-dimethyl-7-nitrobenzofuran-3-one as a residue. The NMR and IR spectra of the same product from a previous run of this reaction were consistent with the proposed structure.

후처리

  1. customwas prepared
  2. temperatureThis mixture was heated
  3. temperatureat reflux for one hour with vigorous stirring
  4. temperatureThe reaction mixture was cooled
  5. extractionextracted three times with methylene chloride
  6. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent was evaporated from the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-f1825f0b5f7f4e1bb24e9f92e97f9cdd
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05521147

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