Phosphorus oxychloride → 2-Chloro-3,5-dinitrobenzonitrile

反応式

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

参加物

反応物 2

HCID 24813Phosphorus oxychloride

HCID 2356272-chloro-3,5-dinitrobenzamide

生成物 1

HCID 42574512-Chloro-3,5-dinitrobenzonitrile

実験手順

A mixture of 31.8 gm. (0.129 mole) of 2-chloro-3,5-dinitrobenzamide and 50 ml. of phosphorous oxychloride is heated under reflux for one hour. The excess phosphorous oxychloride is removed by distillation under reduced pressure. To the residue is cautiously added ice water. The light yellow-green solid is removed by filtration and washed with water. There is obtained 28.0 g. (95%) of material melting at 139°-41°.

後処理

additionA mixture of 31.8 gm
temperatureunder reflux for one hour
customThe excess phosphorous oxychloride is removed by distillation under reduced pressure
customThe light yellow-green solid is removed by filtration
washwashed with water
customThere is obtained 28.0 g

出典と根拠

ORDレコード: ord-a86df7a1b67c46248581de07d0973b98
出典データセット: uspto-grants-1978_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04095028

反応ノート

読み込み中…

参加物