Pentanoic Acid → 2-butyl-1H-imidazo[4,5-b]pyridine

HRID 466668ノート

反応式

HRID 466668 の反応式
[C:1](O)(=O)[CH2:2][CH2:3][CH2:4][CH3:5].[NH2:8][C:9]1[C:14]([NH2:15])=[CH:13][CH:12]=[CH:11][N:10]=1>>[CH2:2]([C:1]1[NH:15][C:14]2[C:9]([N:8]=1)=[N:10][CH:11]=[CH:12][CH:13]=2)[CH2:3][CH2:4][CH3:5]

参加物

3

反応物 2

HCID 7991Pentanoic AcidHCID 99562,3-Diaminopyridine

生成物 1

HCID 124677102-butyl-1H-imidazo[4,5-b]pyridine収率 95%

反応条件

温度
100 °C

実験手順

A mixture of valeric acid (5.50 mL, 50.4 mmol), 2,3-diaminopyridine (5.0 g, 45.8 mmol), and polyphosphoric acid (50 g) was heated to 100° C. with stirring for 5 hours. Basification (NH4OH), extraction (EtOAc, 4×20 mL), drying (K2CO3), and concentration gave 7.61 g (95%) of the title compound as an amorphous tan solid which was judged pure by 1H NMR and tlc (mp ca 80° C. without recrystallization).

後処理

  1. extractionBasification (NH4OH), extraction (EtOAc, 4×20 mL)
  2. customdrying
  3. concentration(K2CO3), and concentration

出典と根拠

ORDレコード
ord-9772170e5e4242dea2570cf892a0aed0
出典データセット
uspto-grants-1992_10
特許番号
US05157026

反応ノート

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