Hydrogen Bromide → HCID 131731313、化合物

HRID 1406034ノート

反応式

HRID 1406034 の反応式
C[O:2][C:3]1[N:8]=[C:7]([C:9]([O:11]C)=[O:10])[CH:6]=[CH:5][C:4]=1[N:13]1[CH:17]=[C:16]([CH3:18])[N:15]=[CH:14]1.[BrH:19]>C(O)(=O)C>[BrH:19].[CH3:18][C:16]1[N:15]=[CH:14][N:13]([C:4]2[C:3](=[O:2])[NH:8][C:7]([C:9]([OH:11])=[O:10])=[CH:6][CH:5]=2)[CH:17]=1

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 67798582Methyl 6-methoxy-5-(4-methyl-1H-imidazol-1-yl)pyridine-2-carboxylate

生成物 1

HCID 131731313HCID 131731313、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of C2 (3.82 g, 15.9 mmol) in acetic acid (30 mL) and aqueous hydrobromic acid (48%, 30 mL) was heated at reflux for 4 hours. The reaction was allowed to cool to room temperature, and then chilled in an ice bath; the resulting precipitate was collected via filtration and washed with ice water (30 mL). Recrystallization from ethanol (20 mL) provided the title compound as a light yellow solid. Yield: 3.79 g, 12.6 mmol, 79%. LCMS m/z 220.1 (M+1). 1H NMR (400 MHz, DMSO-d6) δ 12.6 (ν br s, 1H), 9.58-9.60 (m, 1H), 8.07 (d, J=7.6 Hz, 1H), 7.88-7.91 (m, 1H), 7.09 (d, J=7.4 Hz, 1H), 2.34 (br s, 3H).

後処理

  1. temperatureat reflux for 4 hours
  2. temperaturechilled in an ice bath
  3. filtrationthe resulting precipitate was collected via filtration
  4. washwashed with ice water (30 mL)
  5. customRecrystallization from ethanol (20 mL)

出典と根拠

ORDレコード
ord-a3439376b21941aca129d2ec70d3962e
出典データセット
uspto-grants-2014_12
特許番号
US08916564B2

反応ノート

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