Methyl Lactate → 2-{1-(Methoxycarbonyl)ethoxy}-3-nitropyridine

HRID 1862260ノート

反応式

HRID 1862260 の反応式
[H-].[Na+].Cl[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1.[C:13]([O:18][CH3:19])(=[O:17])[CH:14]([CH3:16])[OH:15]>O1CCOCC1>[CH3:19][O:18][C:13]([CH:14]([O:15][C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1)[CH3:16])=[O:17]

参加物

5

反応物 3

HCID 11040Methyl LactateHCID 24758Sodium hydrideHCID 796132-Chloro-3-nitropyridine

生成物 1

HCID 219335712-{1-(Methoxycarbonyl)ethoxy}-3-nitropyridine収率 73%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.8 g of sodium hydride was added to a mixture of 3.17 g of 2-chloro-3-nitropyridine, 2.19 g of methyl lactate and 20 ml of 1,4-dioxane at 10° C. The mixture was stirred at room temperature for 1.5 hours, then, poured into ice water, and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 3.3 g of 2-{1-(methoxycarbonyl)ethoxy}-3-nitropyridine.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-8c35a9af41644d81880d7f86246997aa
出典データセット
uspto-grants-2003_03
特許番号
US06537948B1

反応ノート

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