HRID404123

反应详情

EQUATION

反应方程式

HRID 404123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

The compound of example 660 (2.5 g, 7.35 mmol); 4,4,5,5-tetramethyl-2-(4-nitrophenyl)-1,3,2-dioxaborolane (2.19 g, 8.82 mmol) and bis-Pinacolato diborane (180 mg, 0.22 mmol) were taken in dry DMF under argon atmosphere. Degassed 2M solution of sodium carbonate (1.94 g, 18.37 mmol) was added and the reaction mixture was heated to 80° C. for 2 h. The reaction mixture was cooled and the solvent was removed by distillation. The residue was taken in water and this aqueous mixture was extracted with ethyl acetate. The crude material was purified through column chromatography (silicagel, 30% dichloromethane in petroleum ether) to afford the title compound.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed by distillation
  4. extractionthis aqueous mixture was extracted with ethyl acetate
  5. customThe crude material was purified through column chromatography (silicagel, 30% dichloromethane in petroleum ether)