反応 #2348132

ord-e23095323371440f92f2bb8219e04c4c

反応方程式

O=C(O)c1ccc(O)cc1
4-hydroxybenzoic acid
Oc1ccc(S)cc1
4-mercaptophenol
O=C(Sc1ccc(O)cc1)c1ccc(O)cc1
4-Hydroxy-thiobenzoic acid S-(4-hydroxy-phenyl)ester
収率 24.4%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvents were removed by evaporation
  2. 2
    その他the residue was purified by column chromatography (hexane-EtOAc 7:1 to 1:1)

実験手順

A PPE (polyphosphate ester) solution (7 mL) was added to a mixture of 4-hydroxybenzoic acid (552 mg, 4 mmol) and 4-mercaptophenol (554 mg, 4.4 mmol). After stirring for 16 h, the solvents were removed by evaporation and the residue was purified by column chromatography (hexane-EtOAc 7:1 to 1:1). 4-Hydroxy-thiobenzoic acid S-(4-hydroxy-phenyl)ester (240 mg, 24%) was obtained as a white solid. MS (ES) m/z: 247.04 (M+1), 167.03, and 122.55. 13C-NMR (DMSO-d6): δ 188.24, 162.85, 158.82, 135.87, 129.59, 127.10, 116.33, 115.72, and 115.34.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07846915B2uspto-grants-2010_12