HRID1678074
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
- 70 °C
PROCEDURE
实验过程
2.4 g (36.9 mmol) of sodium azide were added to 13.5 g (36.9 mmol) of 2-tert-butyl-4-[4-(3-chloropropyl)piperazin-1-yl]-6-(trifluoromethyl)pyrimidine (DE 197 35 410) in 60 ml of N,N-dimethylformamide (DMF), and the mixture was stirred at 70° C. for 3 hours. The reaction mixture was allowed to cool to room temperature, the mixture was poured into saturated brine, and the aqueous mixture was extracted with ethyl acetate. The organic phase was washed three times with an NaCl solution, dried over Na2SO4, filtered to remove the desiccant and concentrated in vacuo. Yield: 13.7 g.
WORKUP
后处理
- temperatureto cool to room temperature
- extractionthe aqueous mixture was extracted with ethyl acetate
- washThe organic phase was washed three times with an NaCl solution
- dry with materialdried over Na2SO4
- filtrationfiltered
- customto remove the desiccant and
- concentrationconcentrated in vacuo