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

HRID 1982680노트

반응식

HRID 1982680 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-2cfb1a5b0eab459ebfbdb997b4016f95
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04596869

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