Hydroxylamine → 5-Hydroxy-2-pyridinecarboxaldehyde

HRID 861750

反応式

HRID 861750 の反応式
N[OH:2].CN(C)[C:5](Cl)=[O:6].[N:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>CC(C)=O>[CH:5]([C:10]1[CH:11]=[CH:12][C:13]([OH:2])=[CH:14][N:9]=1)=[O:6]

参加物

5

反応物 3

HCID 787HydroxylamineHCID 1049PyridineHCID 6598Dimethylcarbamoyl Chloride

生成物 1

HCID 2783895-Hydroxy-2-pyridinecarboxaldehyde収率 30%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

N-[5-(N',N'-Dimethylcarbamoyl)hydroxy-2-pyridine methylene] hydroxylamine. Dimethylcarbamoyl chloride (5.2 mL, 57 mmol) was added to a solution of N-(5-hydroxy-2-pyridinemethylene) hydroxylamine (6.53 g, 47 mmol) in 40 mL of pyridine. It was stirred at room temperature overnight and then the solvent was removed in vacuo, leaving a light green paste. The paste was dissolved in a minimum quantity of acetone and then triturated with ethyl acetate and placed in the freezer overnight. Glassy needles formed and were filtered and washed with ethyl acetate to yield 3.0 g of pure product (30%), m.p. 134°-135° C.

後処理

  1. customthe solvent was removed in vacuo
  2. customleaving a light green paste
  3. customtriturated with ethyl acetate
  4. customplaced in the freezer overnight
  5. customGlassy needles formed
  6. filtrationwere filtered
  7. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-143cf03b4ad742c593059d8405a026ef
出典データセット
uspto-grants-1998_02
特許番号
US05714615

関連ノート

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