HRID595147
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureupon heating
- customa solution was obtained
- temperaturethen cooled to room temperature
- concentrationconcentrated under reduced pressure
- additionSaturated sodium bicarbonate and dichloromethane were added
- customthe organic phase was recovered
- concentrationconcentrated under reduced pressure
- washThe residue was washed in hexanes/ether
- filtrationfiltered