Hydroxyamine hydrochloride → 468068-31-7

HRID 2415760ノート

反応式

HRID 2415760 の反応式
Cl.[NH2:2][OH:3].[Na].[C:5]([C:7]1[CH:12]=[CH:11][N:10]=[C:9]([N:13]([CH3:15])[CH3:14])[CH:8]=1)#[N:6]>CO>[CH3:14][N:13]([CH3:15])[C:9]1[CH:8]=[C:7]([C:5](=[N:2][OH:3])[NH2:6])[CH:12]=[CH:11][N:10]=1

参加物

5

反応物 3

HCID 443297Hydroxyamine hydrochlorideHCID 5360545Sodium2 回HCID 131452572-(Dimethylamino)pyridine-4-carbonitrile

生成物 1

HCID 135741750468068-31-7収率 134.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of hydroxylamine hydrochloride (0.47 g, 7.0 mmol) in methanol (10 mL) was added sodium metal (0.16 g, 7.0 mmol) portionwise. After all the sodium metal had dissolved 4-cyano-2-dimethylaminopyridine (1.0 g, 7.0 mmol) was added and the reaction was heated to reflux for 4 hours. The reaction was cooled to room temperature, filtered to remove precipitated sodium chloride and the filtrate was evaporated to dryness. The residue was dissolved in ethanol in order to crystallise the product but this was unsuccessful, so the solvent was removed in vacuo to give the title compound as a white solid (1.7 g), which was contaminated with ethanol.

後処理

  1. additionwas added
  2. temperaturethe reaction was heated
  3. temperatureto reflux for 4 hours
  4. filtrationfiltered
  5. customto remove
  6. customprecipitated sodium chloride
  7. customthe filtrate was evaporated to dryness
  8. dissolutionThe residue was dissolved in ethanol in order
  9. customto crystallise the product
  10. customthis was unsuccessful, so the solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bcfad0b031824868932357910f929a60
出典データセット
uspto-grants-2004_11
特許番号
US06821972B2

反応ノート

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