HRID1678074

反应详情

EQUATION

反应方程式

HRID 1678074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureto cool to room temperature
  2. extractionthe aqueous mixture was extracted with ethyl acetate
  3. washThe organic phase was washed three times with an NaCl solution
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customto remove the desiccant and
  7. concentrationconcentrated in vacuo