Sodium Hydroxide → 2-(6-Formamidopyridin-2-yl)-2-methoxyiminoacetic acid

HRID 1982680ノート

反応式

HRID 1982680 の反応式
[OH-].[Na+].[CH:3]([NH:5][C:6]1[N:11]=[C:10]([C:12](=O)[C:13]([O:15]CC)=[O:14])[CH:9]=[CH:8][CH:7]=1)=[O:4].Cl.[CH3:20][O:21][NH2:22]>C(O)C>[CH:3]([NH:5][C:6]1[N:11]=[C:10]([C:12](=[N:22][O:21][CH3:20])[C:13]([OH:15])=[O:14])[CH:9]=[CH:8][CH:7]=1)=[O:4]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 521874O-Methylhydroxylamine hydrochlorideHCID 13060174Ethyl 2-(6-formamidopyridin-2-yl)glyoxylate

生成物 1

HCID 543262512-(6-Formamidopyridin-2-yl)-2-methoxyiminoacetic acid収率 60.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2N Sodium hydroxide solution [solvent:water (1 part)+ethanol (4 parts)] (14.87 ml.) was added to a solution of ethyl 2-(6-formamidopyridin-2-yl)glyoxylate (6.00 g.) in ethanol (180 ml.) at room temperature and stirred at the same temperature for 20 minutes. Methoxyamine hydrochloride (2.71 g.) was added to the resultant solution, stirred at room temperature for 1.5 hours and then concentrated to a small volume under reduced pressure. The precipitates were collected by filteration washed with ethyl acetate and water, dissolved in methanol and then treated with activated charcoal. The solution was concentrated under reduced pressure and then the precipitates were collected by filtration to give 2-(6-formamidopyridin-2-yl)-2-methoxyiminoacetic acid (3.63 g.), mp 170° to 171° C. (dec.).

後処理

  1. stirringstirred at room temperature for 1.5 hours
  2. concentrationconcentrated to a small volume under reduced pressure
  3. customThe precipitates were collected by filteration
  4. washwashed with ethyl acetate and water
  5. dissolutiondissolved in methanol
  6. additiontreated with activated charcoal
  7. concentrationThe solution was concentrated under reduced pressure
  8. filtrationthe precipitates were collected by filtration

出典と根拠

ORDレコード
ord-2cfb1a5b0eab459ebfbdb997b4016f95
出典データセット
uspto-grants-1986_06
特許番号
US04596869

反応ノート

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