2-Chloro-3-nitropyridine → HCID 14677546, 화합물

HRID 330537노트

반응식

HRID 330537 반응식
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH3:11][C:12]1[CH:13]=[C:14]([CH2:17][NH2:18])[O:15][CH:16]=1.C(=O)([O-])O.[Na+]>C(O)C>[CH3:11][C:12]1[CH:13]=[C:14]([CH2:17][NH:18][C:2]2[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=2)[O:15][CH:16]=1

참가 물질

5

반응물 3

HCID 796132-Chloro-3-nitropyridineHCID 516892Sodium BicarbonateHCID 146775454-Methyl-2-furanmethanamine

생성물 1

HCID 14677546HCID 14677546, 화합물수율 91.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 10.4 parts of 2-chloro-3-nitropyridine, 8 parts of 4-methyl-2-furanmethanamine, 7.6 parts of sodium hydrogen carbonate and 120 parts of ethanol was stirred overnight at reflux temperature. The reaction mixture was evaporated and the residue was taken up in water. The product was extracted with 1,1'-oxybisethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated, yielding 14.9 parts (91.2%) of N-[(4-methyl-2-furanyl)methyl]-3-nitro-2-pyridinamine as a residue (int. 3).

후처리

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. extractionThe product was extracted with 1,1'-oxybisethane
  4. customThe extract was dried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography over silica gel
  8. customThe pure fractions were collected
  9. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-5453942a16ed458bb7797593304aaba2
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04897401

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