Sodium Methoxide → 1-Methoxy-7-nitroisoquinoline

HRID 1070465ノート

反応式

HRID 1070465 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[CH3:15][O-:16].[Na+]>CO>[CH3:15][O:16][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[CH:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 218626571-chloro-7-nitroisoquinoline

生成物 1

HCID 223970461-Methoxy-7-nitroisoquinoline収率 81%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of 1-chloro-7-nitroisoquinoline (670 mg, 3.21 mmol) obtained in Preparation Example 1-5, Step 4 in methanol (100 ml) was added a 1M solution (6.5 ml, 6.5 mmol) of sodium methoxide. The mixture was refluxed under heating for 3 hr and concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:acetone=30:1) to give 1-methoxy-7-nitroisoquinoline (530 mg, 81%).

後処理

  1. temperatureThe mixture was refluxed
  2. temperatureunder heating for 3 hr
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washwashed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (chloroform:acetone=30:1)

出典と根拠

ORDレコード
ord-eff2d86e147f4a2caef03d3bd8a359b3
出典データセット
uspto-grants-2005_06
特許番号
US06903094B2

反応ノート

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