4-Fluoroaniline → Fluoroimide

HRID 596179

反応式

HRID 596179 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-Fluoroaniline2 回HCID 6437972,3-Dichloromaleic acid

生成物 1

HCID 93228Fluoroimide収率 97.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

10 g (0.06 mol) of 2,3-dichloromaleic acid was dissolved in 100 ml of water. Then, to the resulting solution 5.55g (0.05 mol) of 4-fluoroaniline was added dropwise over a period of 5 min. at reflux temperatures under agitation. Upon addition of 4 -fluoroaniline, a white crystal separated out immediately but the reaction was allowed to preceed for two hours. After cooling, the crystal was separated by filtration and fully rinsed with water to obtain 12.7g (yield, 97.7%) of N-(4-fluorophenyl)-2,3-dichloromaleimide (Sample No. 1) having an average grain size of 10μ. An analysis by gas chromatography showed that the N-(4-fluorophenyl)-2,3-dichloromaleimide had a purity of 96.2%.

後処理

  1. temperatureat reflux temperatures under agitation
  2. customa white crystal separated out immediately
  3. temperatureAfter cooling
  4. customthe crystal was separated by filtration
  5. washfully rinsed with water

出典と根拠

ORDレコード
ord-848a2ba1c81d40caa92dd79dae27eb59
出典データセット
uspto-grants-1977_03
特許番号
US04010182

関連ノート

読み込み中…