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Diethylamine → N,N-Diethyl-2-methyl-5-nitropyridine-3-carboxamide

HRID 972753
笔记
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反应方程式

HRID 972753 反应方程式
[CH3:1][C:2]1[N:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH2:14]([NH:16][CH2:17][CH3:18])[CH3:15]>C(Cl)(Cl)Cl>[CH2:14]([N:16]([CH2:17][CH3:18])[C:4](=[O:6])[C:3]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[N:10][C:2]=1[CH3:1])[CH3:15]
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 8021DiethylamineHCID 2872402-甲基-5-硝基烟酸

产物 1

HCID 21405249N,N-Diethyl-2-methyl-5-nitropyridine-3-carboxamide

试剂、催化剂与溶剂 1

HCID 6212三氯甲烷溶剂

实验过程

In dry chloroform were dissolved 0.3 g of 2-methyl-5-nitronicotinic acid and 1.5 ml of diethylamine. After addition of 10 g of phosphorous pentaoxide, the mixture was stirred with heating at 55° - 60° C. for 3 hours. After cooling, the chloroform portion was separated and evaporated under reduced pressure. The residue was, after addition of water, neutralized with sodium hydrogen carbonate and extracted with ethyl acetate. The extract was concentrated and purified on a silica gel column to give 0.25 g of a colorless oil.

后处理

  1. additionAfter addition of 10 g of phosphorous pentaoxide
  2. temperaturewith heating at 55° - 60° C. for 3 hours
  3. temperatureAfter cooling
  4. customthe chloroform portion was separated
  5. customevaporated under reduced pressure
  6. additionafter addition of water
  7. extractionextracted with ethyl acetate
  8. concentrationThe extract was concentrated
  9. custompurified on a silica gel column

来源与证据

ORD记录
ord-d7b2854d4e034bd0b0ed3318118488d7
来源数据集
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US04053608

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记