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Methanol → 6-Chloro-2-methoxy-3-nitropyridine

HRID 31819
ノート
印刷プレビュー

反応式

HRID 31819 の反応式
[H-].[Na+].[CH3:3][OH:4].Cl[C:6]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[C:8]([Cl:15])[N:7]=1.O>C1(C)C(C)=CC=CC=1>[Cl:15][C:8]1[N:7]=[C:6]([O:4][CH3:3])[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 24758Sodium hydrideHCID 852392,6-Dichloro-3-nitropyridine

生成物 1

HCID 107977036-Chloro-2-methoxy-3-nitropyridine

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒3 回

実験手順

To a suspension of sodium hydride (684 mg, 28.49 mmol) in xylene (100 ml), methanol (0.98 ml, 25.9 mmol) in xylene (30 ml) was added under nitrogen. The mixture was stirred for 20 min. A solution of 2,6-dichloro-3-nitropyridine (5.0 g, 25.9 mmo) in xylene (100 ml) was added to the reaction mixture and stirred at room temperature overnight. Water (50 ml) was added and the organic layer was separated. The organics was washed with water (1×50 ml) and brine (2×50 ml), dried, and concentrated in vacuo. The crude product was purified by flash chromatography (10:1 methylene chloride and acetone) to provide the desired compound, 6-chloro-2-methoxy-3-nitro-pyridine, as the only isomer as light yellow solid (90%).

後処理

  1. additionwas added under nitrogen
  2. stirringstirred at room temperature overnight
  3. customthe organic layer was separated
  4. washThe organics was washed with water (1×50 ml) and brine (2×50 ml)
  5. customdried
  6. concentrationconcentrated in vacuo
  7. customThe crude product was purified by flash chromatography (10:1 methylene chloride and acetone)

出典と根拠

ORDレコード
ord-f960d4a592e84bd0a048645b99309520
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07425557B2

反応ノート

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