Acetone → 3,4-Dimethylhexane-2,5-dione

HRID 2110416ノート

反応式

HRID 2110416 の反応式
[CH3:1][C:2]1[O:3][C:4]([CH3:9])=[C:5]([CH3:8])[C:6]=1[CH3:7].CC(=[O:13])C>>[CH3:7][CH:6]([CH:5]([CH3:8])[C:4](=[O:3])[CH3:9])[C:2](=[O:13])[CH3:1]

参加物

3

反応物 2

HCID 180AcetoneHCID 1391982,3,4,5-Tetramethylfuran

生成物 1

HCID 328513,4-Dimethylhexane-2,5-dione収率 42.5%

実験手順

Compound 219A was made in accordance with the procedures described in Hancock et al. J. Org. Chem. 42,1850-1856 (1977) & Amarnath et al. J. Org. Chem., 60, 301-307 (1995). 2-Propanone (100 mL, 1.1 mol) was refluxed over PbO2 (26.7 g, 0.112 mol) for 28 h. After cooling to rt, the reaction mixture was filtered and the residue was washed with acetone. The filtrate was concentrated under reduced pressure to remove the acetone and then distilled at 20 Torr. The fraction that came over between 100-120° C. was collected to give 6.75 g (42.5%) of 3,4-dimethylhexane-2,5-dione as a light yellow oil.

後処理

  1. filtrationthe reaction mixture was filtered
  2. washthe residue was washed with acetone
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customto remove the acetone
  5. distillationdistilled at 20 Torr
  6. customcame over between 100-120° C.
  7. customwas collected

出典と根拠

ORDレコード
ord-29f0c02771a246868ee7e43af6e97629
出典データセット
uspto-grants-2009_04
特許番号
US07517904B2

反応ノート

読み込み中…