4-Fluoroaniline → Fluoroimide

HRID 596187ノート

反応式

HRID 596187 の反応式
[Cl:1]/[C:2](=[C:6](\[Cl:10])/[C:7](O)=[O:8])/[C:3](O)=[O:4].[F:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1>O>[F:11][C:12]1[CH:18]=[CH:17][C:15]([N:16]2[C:3](=[O:4])[C:2]([Cl:1])=[C:6]([Cl:10])[C:7]2=[O:8])=[CH:14][CH:13]=1

参加物

4

反応物 2

HCID 97314-FluoroanilineHCID 6437972,3-Dichloromaleic acid

生成物 1

HCID 93228Fluoroimide収率 98.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

18.5g (0.1 mol) of 2,3-dichloromaleic acid was dissolved in 120 ml of water. To the resulting solution 8.9g (0.08mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at reflux temperatures under agitation. The mixture was then allowed to react for 2 hours at reflux temperatures. Upon cooling the reaction mixture, precipitated crystal was separated by filtration to obtain 20.3g of N-(4-fluorophenyl)-2,3-dichloromaleimide melting at 239°-240° C (not corrected) at a yield of 98.1%. An analysis by gas chromatography showed the product had a purity of 95.5%.

後処理

  1. temperatureat reflux temperatures under agitation
  2. customto react for 2 hours
  3. temperatureat reflux temperatures
  4. temperatureUpon cooling the reaction mixture
  5. customprecipitated crystal
  6. customwas separated by filtration

出典と根拠

ORDレコード
ord-b1e8f4be274a499cb721d57cde8bddc1
出典データセット
uspto-grants-1977_03
特許番号
US04010182

反応ノート

読み込み中…