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

HRID 1756100ノート

反応式

HRID 1756100 の反応式
[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]

参加物

4

反応物 2

HCID 22172MethoxyacetoneHCID 786452-Hydrazinopyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fdfb30b531b3427497b8373a7e1d2497
出典データセット
uspto-grants-1995_08
特許番号
US05439917

反応ノート

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