Chloral → Acetamide, 2-(hydroxyimino)-N-phenyl-

HRID 1369063

반응식

HRID 1369063 반응식
Cl[C:2](Cl)(Cl)[CH:3]=[O:4].S([O-])([O-])(=O)=O.[Na+].[Na+].Cl[C:15]1[CH:16]=[C:17]([CH:19]=[C:20](Cl)[CH:21]=1)[NH2:18].Cl.[NH2:24][OH:25]>O.Cl>[CH:21]1[CH:20]=[CH:19][C:17]([NH:18][C:3](/[CH:2]=[N:24]/[OH:25])=[O:4])=[CH:16][CH:15]=1

참가 물질

7

반응물 4

HCID 6407ChloralHCID 122813,5-DichloroanilineHCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 6861488Acetamide, 2-(hydroxyimino)-N-phenyl-

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매3회

실험 절차

To a solution of trichloroacetaldehyde monohydate (13.25 g, 1.3 eq) in H2O (150 mL) was successively added sodium sulfate (17.55 g, 4.0 eq), a hot solution (ca. 80° C.) of 3,5-dichloroaniline (10.0 g, 61.5 mmol) in H2O (50 mL) and 37% HCl (6.1 mL), and a solution of hydroxylamine hydrochloride (16.3 g, 3.8 eq) in H2O (75 mL) with rapid stirring. Once the addition was completed the reaction mixture was heated at reflux for 2 minutes and then allowed to cool to room temperature. The resulting light brown precipitate was filtered, washed with H2O (200 mL) and then dried to yield the crude isonitrosoacetanilide (20.13 g).

후처리

  1. additionOnce the addition
  2. temperaturewas heated
  3. temperatureat reflux for 2 minutes
  4. filtrationThe resulting light brown precipitate was filtered
  5. washwashed with H2O (200 mL)
  6. customdried

출처 및 근거

ORD 기록
ord-62e3b4db55134910b92355b50077dc92
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06576656B1

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