HRID1515096

反应详情

EQUATION

反应方程式

HRID 1515096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

3-(tert-Butyldimethylsilyloxy)-1-[4-(3,4-dichlorobenzyloxy)phenyl]propan-1-ol (300 mg, 0.680 mmol) produced in Example 27 (27B), palladium(II) trifluoroacetate (12 mg, 0.036 mmol), and 4,7-diphenyl-1,10-phenanthroline (12 mg, 0.036 mmol) were dissolved in butyl vinyl ether (5 mL), and triethylamine (20 μL, 0.14 mmol) was added thereto, and the resulting mixture was stirred under a nitrogen atmosphere at 80° C. for 4 hours. After cooling to room temperature, the reaction solution was filtered, and the solvent was distilled off under reduced pressure, whereby a crude product was obtained. This crude product was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 96:4 (v/v)), whereby the objective title compound was obtained as a colorless oily substance (275 mg, yield: 87%).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe reaction solution was filtered
  3. distillationthe solvent was distilled off under reduced pressure, whereby a crude product
  4. customwas obtained
  5. customThis crude product was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 96:4 (v/v)), whereby the objective title compound
  6. customwas obtained as a colorless oily substance (275 mg, yield: 87%)