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

반응식

[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]

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 2356272-chloro-3,5-dinitrobenzamide

생성물 1

HCID 42574512-Chloro-3,5-dinitrobenzonitrile

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록: ord-448ea68a55ae4343ab55d2f35901d78c
출처 데이터셋: uspto-grants-1979_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04159278

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