p-Toluenesulfonic acid → 3-[(5,6-Difluoro-2-methyl-4-oxo-4H-chromen-8-yl)methylene]pentane-2,4-dione

HRID 1669762ノート

反応式

HRID 1669762 の反応式
[F:1][C:2]1[C:11]([F:12])=[CH:10][C:9]([CH:13]=O)=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([CH3:15])[O:7]2.[CH3:17][C:18](=[O:23])[CH2:19][C:20](=[O:22])[CH3:21].C1(C)C=CC(S(O)(=O)=O)=CC=1.C(OCC)(=O)C>C1(C)C=CC=CC=1>[F:1][C:2]1[C:11]([F:12])=[CH:10][C:9]([CH:13]=[C:19]([C:18](=[O:23])[CH3:17])[C:20](=[O:22])[CH3:21])=[C:8]2[C:3]=1[C:4](=[O:16])[CH:5]=[C:6]([CH3:15])[O:7]2

参加物

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 8857Ethyl AcetateHCID 31261AcetylacetoneHCID 574388895,6-difluoro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde

生成物 1

HCID 575033293-[(5,6-Difluoro-2-methyl-4-oxo-4H-chromen-8-yl)methylene]pentane-2,4-dione

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

250 mg (1.12 mmol) of 5,6-difluoro-2-methyl-4-oxo-4H-chromene-8-carbaldehyde, 0.14 ml (1.34 mmol) of 2,4-pentanedione and 212.1 mg (1.12 mmol) of para-toluenesulfonic acid are heated in 100 ml of toluene under reflux with a water trap for 10 h. After cooling, 100 ml of ethyl acetate are added, and the reaction mixture is washed with water and with brine. Drying of the organic phase and concentration result in 269.7 mg (79% of theory) of the title compound as beige-coloured crystals.

後処理

  1. temperatureunder reflux with a water trap for 10 h
  2. temperatureAfter cooling
  3. washthe reaction mixture is washed with water and with brine
  4. customDrying of the organic phase and concentration

出典と根拠

ORDレコード
ord-bb471bf970f44329b7fbb06869ef416b
出典データセット
uspto-grants-2011_08
特許番号
US07989633B2

反応ノート

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