HRID2097697

反应详情

EQUATION

反应方程式

HRID 2097697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4,4,5,5-tetramethyl-2-(2-(2,4,6-trimethoxybenzylthio)phenyl)-1,3,2-dioxaborolane (1.2 g, 2.9 mmol), 3-lodophenol (0.65 g, 2.9 mmol), Ag2CO3 (0.82 g, 2.9 mmol) and Pd(PPh3)4 (0.16 g, 0.15 mmol) in 6 ml of THF was refluxed in the dark for 12 h. The reaction mixture was poured into H2O and the resulting mixture extracted with ether. The organic layer was washed with brine (3×20 ml) and dried over MgSO4 and concentrated. The residue was purified by silica flash chromatography (40/60, ethylacetate/hexane) to afford 2′-(2,4,6-trimethoxybenzylthio)biphenyl-3-ol.

WORKUP

后处理

  1. temperaturewas refluxed in the dark for 12 h
  2. extractionthe resulting mixture extracted with ether
  3. washThe organic layer was washed with brine (3×20 ml)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue was purified by silica flash chromatography (40/60, ethylacetate/hexane)