2,3,4,5-Tetrafluoroaniline → HCID 18948775、化合物
反応式
[F:1][C:2]1[C:8]([F:9])=[C:7]([F:10])[C:6]([F:11])=[CH:5][C:3]=1[NH2:4].Cl[S:13]([OH:16])(=[O:15])=[O:14]>ClC(Cl)=C(Cl)Cl>[NH2:4][C:3]1[C:2]([F:1])=[C:8]([F:9])[C:7]([F:10])=[C:6]([F:11])[C:5]=1[S:13]([OH:16])(=[O:15])=[O:14]参加物
4
実験手順
2,3,4,5-Tetrafluoroaniline (16.5 g, 0.1 mol) was added dropwise over 20 minutes with stirring to a mixture of chlorosulfonic acid (14 g, 0.12 mol) in tetrachloroethylene (100 mL) with ice bath cooling. A yellow precipitate formed immediately.. When the addition was complete, the mixture was heated at reflux for three hours, during which a light tan granular solid formed. The solid was collected by filtration, washed with ether, and dried in vacuo to give the title compound (25 g); m.p. 272°-276° .
後処理
- temperaturecooling
- customA yellow precipitate formed immediately
- additionWhen the addition
- temperaturethe mixture was heated
- temperatureat reflux for three hours, during which a light tan granular solid
- customformed
- filtrationThe solid was collected by filtration
- washwashed with ether
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-bf96309d6d084c3ebfda1d75022c01d7
- 出典データセット
- uspto-grants-1995_01
- 特許番号
- US05378704
反応ノート
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