Hydrochloric Acid → 4-Methoxyisonitrosoacetanilide

HRID 24318

反応式

HRID 24318 の反応式
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.Cl.[NH2:9][OH:10].[CH3:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][CH:14]=1.Cl>O.S([O-])([O-])(=O)=O.[Na+].[Na+]>[N:9](=[CH:2][C:3]([NH:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][CH3:11])=[CH:14][CH:15]=1)=[O:5])[OH:10]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 7732P-AnisidineHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 67107914-Methoxyisonitrosoacetanilide収率 85.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 24436Sodium Sulfate溶媒

反応条件

温度
60 °C

実験手順

Chloral hydrate (9.6 g) was dissolved in 200 mL of water containing 83 g of sodium sulfate. The solution was warmed to 60° C., a solution of 11.4 g of hydroxylamine hydrochloride in 50 mL of water was added and the mixture was held at 60° C. In a separate flask, 6.4 g of 4-anisidine and 4.3 mL of concentrated hydrochloric acid in 80 mL of water was warmed to 80° C. The first solution was added to the second and the mixture refluxed for 2 minutes after which it was cooled slowly to room temperature and then cooled in an ice bath. The tan precipitate was collected by vacuum filtration, washed with water and dried under vacuum to give 8.6 g (85% yield) of N-(2-hydroximino-acetyl)anisidine.

後処理

  1. customwas held at 60° C
  2. additionThe first solution was added to the second and the mixture
  3. temperaturerefluxed for 2 minutes after which it
  4. temperaturewas cooled slowly to room temperature
  5. temperaturecooled in an ice bath
  6. filtrationThe tan precipitate was collected by vacuum filtration
  7. washwashed with water
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-6aec756dbaea426a847093dad6f4cd85
出典データセット
uspto-grants-2005_02
特許番号
US06855730B2

関連ノート

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