Methoxyacetone → 3-Methoxy-2-methyl-1H-pyrrolo[2,3-b]pyridine

HRID 1756100노트

반응식

HRID 1756100 반응식
[NH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)N.[CH3:9][O:10][CH2:11][C:12](=O)[CH3:13]>C(O)C>[CH3:9][O:10][C:11]1[C:8]2[C:3](=[N:4][CH:5]=[CH:6][CH:7]=2)[NH:1][C:12]=1[CH3:13]

참가 물질

4

반응물 2

HCID 22172MethoxyacetoneHCID 786452-Hydrazinopyridine

생성물 1

HCID 199168183-Methoxy-2-methyl-1H-pyrrolo[2,3-b]pyridine수율 41%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 7,4 g (68 mmol) 2-hydrazinopyridine and 6,0 g (68 mmol) methoxyaceton in 50 ml of ethanol was refluxed for 1 h. The solvent was removed under reduced pressure. The resulting oil was dissolved in diethylene glycol and refluxed for 1,5 h. The mixture was allowed to cool and was poured into ice-water. Extraction with methylene chloride gave an black oily residue which was treated with boiling petroleumether (60-80). After decanting the solvent was allowed to cool and the precipitated product filtered of affording 4,5 g (41%) pure title compound as a yellow solid.

후처리

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe resulting oil was dissolved in diethylene glycol
  3. temperaturerefluxed for 1,5 h
  4. temperatureto cool
  5. additionwas poured into ice-water
  6. extractionExtraction with methylene chloride
  7. customgave an black oily residue which
  8. additionwas treated
  9. customAfter decanting the solvent
  10. temperatureto cool
  11. filtrationthe precipitated product filtered

출처 및 근거

ORD 기록
ord-fdfb30b531b3427497b8373a7e1d2497
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05439917

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