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

HRID 1075253노트

반응식

HRID 1075253 반응식
[OH-:1].[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.[NH2:20]O>C(O)C>[CH:3]([NH:5][C:6]1[N:11]=[C:10]([C:12](=[N:20][OH:1])[C:13]([OH:15])=[O:14])[CH:9]=[CH:8][CH:7]=1)=[O:4]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 13060174Ethyl 2-(6-formamidopyridin-2-yl)glyoxylate

생성물 1

HCID 1363356462-(6-Formamidopyridin-2-yl)-2-hydroxyiminoacetic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1 N Sodium hydroxide (27.5 ml.) was added to a stirred solution of ethyl 2-(6-formamidopyridin-2-yl)glyoxylate (5.55 g.) in ethanol (100 ml.) at room temperature, and the solution was stirred at the same temperature for 30 minutes. To the solution was added hydroxylamine hydrochloride (1.9 g.) all at once, and the solution was stirred at room temperature for 2 hours. After removing ethanol from the resultant solution under reduced pressure, ethylacetate was added to the residue, and then the solution was adjusted to pH 7 with an aqueous solution of sodium bicarbonate. The aqueous layer was separated and adjusted to pH 2 with 10% hydrochloric acid. The precipitates were collected by filtration, washed with water and dried to give 2-(6-formamidopyridin-2-yl)-2-hydroxyiminoacetic acid (3.6 g.), mp 190° to 192° C. (dec.).

후처리

  1. stirringwas stirred at room temperature for 2 hours
  2. customAfter removing ethanol from the resultant solution under reduced pressure, ethylacetate
  3. additionwas added to the residue
  4. customThe aqueous layer was separated
  5. filtrationThe precipitates were collected by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-f81ef028abbb4ab9ba7e72e680d8e890
출처 데이터셋
uspto-grants-1983_07
특허 번호
US04395411

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