3-Chloro-p-toluonitrile → 3-(2-chloro-6-fluorophenyl)-5-(3-chloro-4-methylphenyl) 1-methyl-1H-1,2,4-triazole

HRID 52242

Reaktionsgleichung

[CH3:1][N:2](S(C1C=CC(C)=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([F:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[Cl:24][C:25]1[CH:26]=[C:27]([CH:30]=[CH:31][C:32]=1[CH3:33])[C:28]#[N:29].[Cl-].[Al+3].[Cl-].[Cl-]>ClC1C=CC=CC=1Cl>[Cl:12][C:6]1[CH:7]=[CH:8][CH:9]=[C:10]([F:11])[C:5]=1[C:4]1[N:29]=[C:28]([C:27]2[CH:30]=[CH:31][C:32]([CH3:33])=[C:25]([Cl:24])[CH:26]=2)[N:2]([CH3:1])[N:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 140 °C

Versuchsvorschrift

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (7.50 g), 3-chloro-4-methylbenzonitrile (3.33 g), anhydrous aluminum chloride (3.00 g) and o-dichlorobenzene (20 ml) is stirred at an oil bath temperature of 140° C. for 1 hour. After cooling, it is washed with saline. Then, it is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexane-ethyl acetate as eluent to give 3.70 g of desired compound.

Aufarbeitung

temperatureAfter cooling
washit is washed with saline
dry with materialThen, it is dried over anhydrous magnesium sulfate
concentrationconcentrated under reduced pressure
customThe concentrate is purified by silica gel column chromatography
additionusing mixed solvent of hexane-ethyl acetate as eluent

Quellen und Nachweise

ORD-Eintrag: ord-d09da8cf964749938e77b8540c98d8c7
Quelldatensatz: uspto-grants-1997_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05616594

Verknüpfte Notizen

Wird geladen…