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

HRID 972753ノート

反応式

HRID 972753 の反応式
[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]

参加物

4

反応物 2

HCID 8021DiethylamineHCID 2872402-Methyl-5-nitropyridine-3-carboxylic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d7b2854d4e034bd0b0ed3318118488d7
出典データセット
uspto-grants-1977_10
特許番号
US04053608

反応ノート

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