六水硝酸铽 → 4-硝基-2,3,5-三甲基吡啶-N-氧化物

HRID 31721

反应方程式

HRID 31721 反应方程式
S(=O)(=O)(O)O.[CH3:6][C:7]1[C:12]([CH3:13])=[CH:11][C:10]([CH3:14])=[CH:9][N+:8]=1[O-:15].[N+:16]([O-])([OH:18])=[O:17].C(=O)([O-])O.[NH4+]>O>[CH3:6][C:7]1[C:12]([CH3:13])=[C:11]([N+:16]([O-:18])=[O:17])[C:10]([CH3:14])=[CH:9][N+:8]=1[O-:15]

参与物

6

反应物 4

HCID 944六水硝酸铽HCID 1118四氧化硫HCID 14013碳酸氢铵HCID 104869072,3,5-三甲基吡啶氧化物

产物 1

HCID 112176114-硝基-2,3,5-三甲基吡啶-N-氧化物收率 81.5%

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

反应条件

温度
85 °C

实验过程

To 98% sulfuric acid (4.93 kg, 49.3 mol), 2,3,5-trimethylpyridine1-oxide (1.38 kg, 10.1 mol) was added. After 97% nitric acid (1.44 kg) was added dropwise thereto over 50 minutes, the mixture was heated at 85° C. for 4 hours. The reaction mixture was poured to a mixture of ammonium hydrogen carbonate (10.6 kg) and water (9.0 L). The mixture was extracted with ethyl acetate (3.0 L×3). The obtained organic layer was concentrated and dried under vacuum overnight to obtain a desired product (1.50 kg).

后处理

  1. extractionThe mixture was extracted with ethyl acetate (3.0 L×3)
  2. concentrationThe obtained organic layer was concentrated
  3. customdried under vacuum overnight

来源与证据

ORD记录
ord-96c5b1cc39524b49a713b86ca5077f65
来源数据集
uspto-grants-2008_09
专利号
US07425634B2

关联笔记

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