HRID595147

反应详情

EQUATION

反应方程式

HRID 595147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

was added to a solution of 3-bromo-5-nitroaniline (3.4 g, 15.7 mmol) and 2-chloro-4-(trifluoromethyl)pyrimidine) (2.27 mL, 18.80 mmol) in dioxane (78 ml) at room temperature, under nitrogen. The mixture became heterogeneous instantly and upon heating, a solution was obtained. The mixture was stirred at 100° C. for 18 hours then cooled to room temperature and concentrated under reduced pressure. Saturated sodium bicarbonate and dichloromethane were added, the organic phase was recovered using a phase separator and then concentrated under reduced pressure. The residue was washed in hexanes/ether and filtered to afford N-(3-bromo-5-nitrophenyl)-4-(trifluoromethyl)pyrimidin-2-amine.

WORKUP

后处理

  1. temperatureupon heating
  2. customa solution was obtained
  3. temperaturethen cooled to room temperature
  4. concentrationconcentrated under reduced pressure
  5. additionSaturated sodium bicarbonate and dichloromethane were added
  6. customthe organic phase was recovered
  7. concentrationconcentrated under reduced pressure
  8. washThe residue was washed in hexanes/ether
  9. filtrationfiltered