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

HRID 1369063

反応式

HRID 1369063 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒3 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-62e3b4db55134910b92355b50077dc92
出典データセット
uspto-grants-2003_06
特許番号
US06576656B1

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