Hydroxyamine hydrochloride → 468068-31-7

HRID 2415760노트

반응식

HRID 2415760 반응식
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

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 5360545Sodium2회HCID 131452572-(Dimethylamino)pyridine-4-carbonitrile

생성물 1

HCID 135741750468068-31-7수율 134.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bcfad0b031824868932357910f929a60
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06821972B2

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