Hydrochloric Acid → N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide

HRID 1449555

반응식

HRID 1449555 반응식
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.S([O-])([O-])(=O)=O.[Na+].[Na+].[CH3:15][C:16]1[CH:17]=[C:18]([CH:20]=[C:21]([CH3:23])[CH:22]=1)[NH2:19].Cl.Cl.[NH2:26][OH:27]>O>[CH3:15][C:16]1[CH:17]=[C:18]([NH:19][C:3](=[O:5])[CH:2]=[N:26][OH:27])[CH:20]=[C:21]([CH3:23])[CH:22]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 79493,5-DimethylanilineHCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 53405864N-(3,5-dimethylphenyl)-2-(hydroxyimino)acetamide수율 95%

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

To a solution of chloral hydrate (14.1 g, 85.24 mM) and sodium sulfate (88.2g, 7.53 eq.) in 270 mL of water was added a solution of 3,5-dimethylaniline in a solution of concentrated HCl (16 mL) and water (51 mL), whereupon an off-white precipitate formed. The mixture was stirred for 10 min prior to adding an aqueous solution of hydroxylamine hydrochloride (17.4 g, 250 mM) in water (50 mL) and then heated at reflux for 10 min during which time the solids dissolved and a tan precipitate formed. The mixture was cooled and filtered, and the collected solids were air dried to yield the title compound (15.0 g, 95%).

후처리

  1. customwhereupon an off-white precipitate formed
  2. temperatureheated
  3. temperatureat reflux for 10 min during which time the solids
  4. dissolutiondissolved
  5. customa tan precipitate formed
  6. temperatureThe mixture was cooled
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-d55d3fed20f641cea9f4145d448636da
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599814

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