Dimethylformamide → (5-Hydroxy-4-oxo-4h-pyran-2-yl)methyl 2-hydroxybenzoate

HRID 259842

反応式

HRID 259842 の反応式
[C:1]([O-:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[Na+].[CH:12]1[C:17](=[O:18])[C:16]([OH:19])=[CH:15][O:14][C:13]=1[CH2:20]Cl.CN(C)C=O>C(OCC)(=O)C>[OH:4][C:3]1[CH:5]=[CH:6][CH:7]=[CH:8][C:2]=1[C:1]([O:10][CH2:20][C:13]1[O:14][CH:15]=[C:16]([OH:19])[C:17](=[O:18])[CH:12]=1)=[O:9]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 82051Chlorokojic acidHCID 16760658Sodium Salicylate

生成物 1

HCID 15307522(5-Hydroxy-4-oxo-4h-pyran-2-yl)methyl 2-hydroxybenzoate収率 58%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
110 °C

実験手順

1 g(6.2 mmole) of sodium salicylate and 0.9 g(15.6 mmole) of chlorokojic acid were dissolved into 70 ml of N,N-dimethylformamide. The resulting solution was heated with stirring for 2 hours in an oil bath of 110° C. After distillating solvent, the residue was dissolved in 300 ml of ethyl acetate. The ethyl acetate solution was washed with 5% chloric acid and distilled water, dried over magnesium sulfate, decolored with active charcoal and filtered. The filtrate was concentrated to give 0.85 g(58%) of 2-(2-hydroxybenzoyl) oxymethyl-5-hydroxy-4H-pyran-4-one as a solid.

後処理

  1. temperatureThe resulting solution was heated
  2. washThe ethyl acetate solution was washed with 5% chloric acid
  3. distillationdistilled water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-4085457d22124f48be4dd9f74eb7d7bb
出典データセット
uspto-grants-1996_06
特許番号
US05523421

関連ノート

読み込み中…