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

HRID 972753노트

반응식

HRID 972753 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7b2854d4e034bd0b0ed3318118488d7
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04053608

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