HRID255341

反应详情

EQUATION

反应方程式

HRID 255341 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

A mixture of acetamide (2.8 g, 47.2 mmol), palladium acetate (0.50 g, 0.80 mmol), XANTPHOS (0.68 g, 1.2 mmol) and cesium carbonate (18 g, 55.2 mmol) was degassed and purged with nitrogen twice. Dry dioxane (50 mL) was added followed by 1,3-dibromo-5-fluorobenzene (10 g, 39.4 mmol). The reaction was heated to 105° C. overnight and then allowed to cool to room temperature. Dichloromethane was added and the mixture was stirred vigorously for 1 hr. The mixture was filtered. The filtrate was concentrated to dryness. Chromatography on silica gel with 25% ethyl acetate in hexanes gave 4.0 g (44%) of the product as a colorless solid.

WORKUP

后处理

  1. customwas degassed
  2. custompurged with nitrogen twice
  3. additionDry dioxane (50 mL) was added
  4. temperatureto cool to room temperature
  5. filtrationThe mixture was filtered
  6. concentrationThe filtrate was concentrated to dryness