乙酰胺 → N-Acetyl-5-nitropyridine-3-carboxamide

HRID 972756笔记

反应方程式

HRID 972756 反应方程式
[C:1]([NH2:4])(=[O:3])[CH3:2].[H-].[Na+].[N+:7]([C:10]1[CH:11]=[N:12][CH:13]=[C:14]([CH:18]=1)[C:15](Cl)=[O:16])([O-:9])=[O:8]>CN(C)C=O>[C:1]([NH:4][C:15](=[O:16])[C:14]1[CH:18]=[C:10]([N+:7]([O-:9])=[O:8])[CH:11]=[N:12][CH:13]=1)(=[O:3])[CH3:2]

参与物

5

反应物 3

HCID 178乙酰胺HCID 24758氢化钠HCID 214053565-Nitro-3-pyridinecarbonyl chloride

产物 1

HCID 21405283N-Acetyl-5-nitropyridine-3-carboxamide收率 6.8%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

In 10 ml of dimethylformamide was dissolved 0.29 g of acetamide, and to this solution was added 0.24 g of NaH (mineral oil 50%). The mixture was then stirred at room temperature for 2 hours. To the mixture was added 0.93 g of 5-nitronicotinic acid chloride, and this was stirred overnight at room temperature. The solvent was evaporated under reduced pressure. The obtained residue was, after addition of water, extracted with ethyl acetate. The extract was dried over sodium sulfate and evaporated to remove the solvent. The obtained product was purified on a silica gel column and recrystallized from ethyl acetate - petroleum ether to give 0.07 g of the desired compound melting at 162° - 163° C.

后处理

  1. stirringthis was stirred overnight at room temperature
  2. customThe solvent was evaporated under reduced pressure
  3. additionafter addition of water
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried over sodium sulfate
  6. customevaporated
  7. customto remove the solvent
  8. customThe obtained product was purified on a silica gel column
  9. customrecrystallized from ethyl acetate - petroleum ether

来源与证据

ORD记录
ord-ae0de909014c4e499ac07a9b8371cecf
来源数据集
uspto-grants-1977_10
专利号
US04053608

反应笔记

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