Chloral Hydrate → N-(2-fluorophenyl)-2-(hydroxyimino)acetamide

HRID 1982601

反応式

HRID 1982601 の反応式
[F:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH2:4].Cl.[NH2:10][OH:11].S([O-])([O-])(=O)=O.[Na+].[Na+].Cl[C:20](Cl)(Cl)[CH:21]([OH:23])O>Cl.O>[F:1][C:2]1[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=1[NH:4][C:21](=[O:23])[CH:20]=[N:10][OH:11]

参加物

7

反応物 4

HCID 2707Chloral HydrateHCID 95842-FluoroanilineHCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 6710880N-(2-fluorophenyl)-2-(hydroxyimino)acetamide収率 87.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒4 回

反応条件

温度
25 °C

実験手順

A solution of 39.4 g of 2-fluoroaniline in 32.4 ml of concentrated hydrochloric acid and 215 ml of water and then a solution of 77.6 g of hydroxylamine hydrochloride in 355 ml of water were added to a mixture of 886 g of sodium sulfate hydrated with 10 moles of water, 64.55 g of chloral hydrate and 850 ml of water and the mixture was heated to reflux with stirring over 45 minutes and reflux was maintained for 5 minutes. The mixture was cooled to 25° C. and held there for 45 minutes. The product was washed with water and dried at room temperature and then at 70° C. under reduced pressure to obtain 56.8 g of N-(2-fluorophenyl)-2-hydroxyimino-acetamide melting at 120° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux
  3. temperaturereflux
  4. temperaturewas maintained for 5 minutes
  5. waitheld there for 45 minutes
  6. washThe product was washed with water
  7. customdried at room temperature

出典と根拠

ORDレコード
ord-21c9014cb781456591a5f8798fba3919
出典データセット
uspto-grants-1986_06
特許番号
US04596875

関連ノート

読み込み中…