HRID249410

反应详情

EQUATION

反应方程式

HRID 249410 的结构方程式

PROCEDURE

实验过程

2.3 g (0.093 mol) of 97% sodium hydride were added a little at a time to 300 ml of ethanol at 20°-35° C. and dissolved by stirring for 15 minutes. Then, while stirring at 0° C., 18.5 g (0.093 mol) of 2-amino-4-fluoro-6-trifluoromethoxy-1,3,5-triazine were added over the course of 10 minutes, and the mixture was stirred at 0° C. for 1 hour and at 22° C. overnight. The residue from concentration under reduced pressure was taken up in methylene chloride, extracted with water and dried. Concentration yielded 17.9 g (85.9% of theory) of the title compound of melting point 69°-71° C.

WORKUP

后处理

  1. dissolutiondissolved
  2. stirringThen, while stirring at 0° C.
  3. stirringthe mixture was stirred at 0° C. for 1 hour and at 22° C. overnight
  4. concentrationThe residue from concentration under reduced pressure
  5. extractionextracted with water
  6. customdried
  7. concentrationConcentration