六水硝酸铽 → 1-(2-Chloro-4-fluoro-5-nitrophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

HRID 1465

反应方程式

HRID 1465 反应方程式
[N+:1]([O-:4])(O)=[O:2].[Cl:5][C:6]1[CH:11]=[C:10]([F:12])[CH:9]=[CH:8][C:7]=1[N:13]1[C:18](=[O:19])[NH:17][C:16](=[O:20])[N:15]([CH3:21])[C:14]1=[O:22]>S(=O)(=O)(O)O>[Cl:5][C:6]1[CH:11]=[C:10]([F:12])[C:9]([N+:1]([O-:4])=[O:2])=[CH:8][C:7]=1[N:13]1[C:18](=[O:19])[NH:17][C:16](=[O:20])[N:15]([CH3:21])[C:14]1=[O:22]

参与物

4

反应物 2

HCID 944六水硝酸铽HCID 572686601-(2-chloro-4-fluorophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione

产物 1

HCID 572803321-(2-Chloro-4-fluoro-5-nitrophenyl)-3-methyl-s-triazine-2,4,6(1H,3H,5H)-trione收率 75.6%

试剂、催化剂与溶剂 1

HCID 1118四氧化硫溶剂

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.).

后处理

  1. temperaturewhile maintaining the reaction mixture temperature below 10° C
  2. additionAfter the addition
  3. temperaturecooled to 10° C
  4. filtrationThe resultant aqueous mixture is filtered
  5. customto obtain a solid which
  6. washis washed with water
  7. customair-dried

来源与证据

ORD记录
ord-e4418b697e514e7891fd2f8cc0451b85
来源数据集
uspto-grants-1998_03
专利号
US05726126

关联笔记

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