Potassium Carbonate → 3-(4-Nitrophenyl)pentane-2,4-dione

HRID 450089

반응식

HRID 450089 반응식
[CH3:1][C:2](=[O:7])[CH2:3][C:4](=[O:6])[CH3:5].I[C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O.O>[N+:15]([C:12]1[CH:13]=[CH:14][C:9]([CH:3]([C:2](=[O:7])[CH3:1])[C:4](=[O:6])[CH3:5])=[CH:10][CH:11]=1)([O-:17])=[O:16]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 124951-Iodo-4-nitrobenzeneHCID 31261Acetylacetone

생성물 1

HCID 35304123-(4-Nitrophenyl)pentane-2,4-dione수율 60.4%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

A mixture of pentane-2,4-dione (4.41 g, 40 mmol), 1-iodo-4-nitrobenzene (5 g, 20 mmol) and potassium carbonate (11 g, 80 mmol) were heated in DMSO (15 ml) at 120° C. for 3 hr. The reaction mixture was cooled to room temperature, diluted with water (100 ml), and then extracted with ethyl acetate. The organic layer was washed with water, brine and dried. Evaporation gave a residue which was chromatographed over silica gel eluting with ethyl acetate/pet ether (5:95) to give 3-(4-nitrophenyl)-pentane-2,4-dione (2.67 g, 60%) as solid.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water, brine
  3. customdried
  4. customEvaporation
  5. customgave a residue which
  6. customwas chromatographed over silica gel eluting with ethyl acetate/pet ether (5:95)

출처 및 근거

ORD 기록
ord-358a4571793c4c279af155eb1a9e2225
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486962B2

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