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

HRID 493956ノート

反応式

HRID 493956 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

First, 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., and the mixture was stirred at room temperature for 1.5 hours. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and then concentrated. The residue was subjected to silica gel column chromatography to give 3.3 g of 2-{1-(methoxycarbonyl)ethoxy}-3-nitropyridine.

後処理

  1. extractionthe mixture was extracted 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-f2a80b2b51c44c3fa1378f79eec0efab
出典データセット
uspto-grants-2009_05
特許番号
US07538072B2

反応ノート

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