Isobutylamine → 5-Methyl-7-isobutylamino-1H-pyrazolo[4,3-b]pyridine

HRID 637985ノート

反応式

HRID 637985 の反応式
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]2[CH:9]=[N:10][NH:11][C:3]=12.[CH2:12]([NH2:16])[CH:13]([CH3:15])[CH3:14]>O.C(O)C>[CH3:8][C:6]1[N:5]=[C:4]2[CH:9]=[N:10][NH:11][C:3]2=[C:2]([NH:16][CH2:12][CH:13]([CH3:15])[CH3:14])[CH:7]=1

参加物

5

反応物 2

HCID 6558IsobutylamineHCID 116798717-Chloro-5-methyl-1H-pyrazolo[4,3-b]pyridine

生成物 1

HCID 202548525-Methyl-7-isobutylamino-1H-pyrazolo[4,3-b]pyridine収率 40.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of 7-chloro-5-methyl-1H-pyrazolo[4,3-b]pyridine (1.0 g, 0.006 mole) and isobutylamine (58 g) in water (100 ml) and ethanol (50 ml) was heated under reflux for 10 days. The reaction mixture was cooled and evaporated to dryness. The oily residue was basified to pH8-9 with 10% sodium carbonate solution. The residue was extracted with ethyl acetate (3×100 ml), dried (Na2SO4) and evaporated to dryness to give a yellow oil. This was purified by column chromatography on alumina, and eluted with chloroform/methanol to give the desired compound as a white solid (500 mg). m.p. 162°-164° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 10 days
  3. temperatureThe reaction mixture was cooled
  4. customevaporated to dryness
  5. extractionThe residue was extracted with ethyl acetate (3×100 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated to dryness
  8. customto give a yellow oil
  9. customThis was purified by column chromatography on alumina
  10. washeluted with chloroform/methanol

出典と根拠

ORDレコード
ord-1e35a82176b84261aec90207eee6f937
出典データセット
uspto-grants-1985_12
特許番号
US04559348

反応ノート

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