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

HRID 450089

反応式

HRID 450089 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-358a4571793c4c279af155eb1a9e2225
出典データセット
uspto-grants-2013_07
特許番号
US08486962B2

関連ノート

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