反应 #1561

ord-e4418b697e514e7891fd2f8cc0451b85

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度while maintaining the reaction mixture temperature below 10° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    温度cooled to 10° C
  4. 4
    过滤The resultant aqueous mixture is filtered
  5. 5
    其他to obtain a solid which
  6. 6
    洗涤is washed with water
  7. 7
    其他air-dried

实验过程

Nitric acid (70% real, 8.3 mL, 0.131 mol) is added to a solution of 1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione (32.4 g, 0.119 mol) in concentrated sulfuric acid while maintaining the reaction mixture temperature below 10° C. After the addition is complete, the reaction mixture is stirred at room temperature for 30 minutes, cooled to 10° C and diluted with ice-water. The resultant aqueous mixture is filtered to obtain a solid which is washed with water and air-dried to give the title product as a white solid (28.5 g, mp 135°-139° C.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05726126uspto-grants-1998_03