Thiophenol → HCID 402511、化合物

HRID 276974ノート

反応式

HRID 276974 の反応式
Cl[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=2[CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[C:25]1([SH:31])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(O)C>[C:25]1([S:31][CH2:2][C:3]2[CH:4]=[CH:5][C:6]3[O:11][C:10](=[O:12])[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:8][C:7]=3[CH:18]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 10659438Ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate

生成物 1

HCID 402511HCID 402511、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1 g of ethyl 6-chloromethyl-2-oxo-2H-1-benzopyran-3-carboxylate (3.75 mmol), 0.57 g of potassium carbonate (4.13 mmol), 2.07 g of thiophenol (18.75 mmol) and 10 ml of absolute ethanol is reflux for 3 h. After removal of the solvent by distillation under reduced pressure, the residue is taken up in chloroform. The organic phase is washed with water and then dried over MgSO4. The solvent is removed by distillation under reduced pressure and the residue is washed with hexane to remove the excess thiophenol. The title product is recrystallized from ethyl acetate/petroleum ether.

後処理

  1. temperatureis reflux for 3 h
  2. customAfter removal of the solvent
  3. distillationby distillation under reduced pressure
  4. washThe organic phase is washed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent is removed by distillation under reduced pressure
  7. washthe residue is washed with hexane
  8. customto remove the excess thiophenol
  9. customThe title product is recrystallized from ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-bc3cf4d6f6734b04aa103da6ccae100d
出典データセット
uspto-grants-2002_03
特許番号
US06355658B1

反応ノート

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