반응 #1561

ord-e4418b697e514e7891fd2f8cc0451b85

반응 방정식

O=[N+]([O-])O
Nitric acid
Cn1c(=O)[nH]c(=O)n(-c2ccc(F)cc2Cl)c1=O
1-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione
Cn1c(=O)[nH]c(=O)n(-c2cc([N+](=O)[O-])c(F)cc2Cl)c1=O
title product
수율 75.6%
Cn1c(=O)[nH]c(=O)n(-c2cc([N+](=O)[O-])c(F)cc2Cl)c1=O
1-(2-Chloro-4-fluoro-5-nitrophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione
수율 75.6%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while maintaining the reaction mixture temperature below 10° C
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    온도cooled to 10° C
  4. 4
    여과The resultant aqueous mixture is filtered
  5. 5
    기타to obtain a solid which
  6. 6
    세척is washed with water
  7. 7
    기타air-dried

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726126uspto-grants-1998_03