Phosphorus oxychloride → 2,4-Dichloro-3,5-dinitrobenzonitrile

反応式

[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]([NH2:6])=O.P(Cl)(Cl)(Cl)=O>>[Cl:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[C:9]([Cl:14])[C:8]([N+:15]([O-:17])=[O:16])=[CH:7][C:3]=1[C:4]#[N:6]

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 964252,4-Dichloro-3,5-dinitrobenzamide

生成物 1

HCID 987512,4-Dichloro-3,5-dinitrobenzonitrile

実験手順

A mixture of 66.0 gm. (0.235 mole) of 2,4-dichloro-3,5-dinitrobenzamide and 140 ml. of phosphorus oxychloride is heated at reflux for one hour. The solution is cooled to room temperature. The excess phosphorus oxychloride is distilled off in vacuo. The solid residue is triturated with ice-water and filtered. There is obtained 54.0 g. (88%) of a tan solid melting at 139°-141°.

後処理

additionA mixture of 66.0 gm
temperatureat reflux for one hour
distillationThe excess phosphorus oxychloride is distilled off in vacuo
customThe solid residue is triturated with ice-water
filtrationfiltered
customThere is obtained 54.0 g

出典と根拠

ORDレコード: ord-87b4173c935e4915aae7b0d1d29b4574
出典データセット: uspto-grants-1979_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04169153

反応ノート

読み込み中…

参加物