Reaktionsgleichung
[CH3:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([CH3:10])[CH:9]=1)[CH:5]=[O:6].[Cl:11]C1C=CC=CC=1Cl>>[CH3:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([CH3:10])[CH:9]=1)[C:5]([Cl:11])=[O:6]Komponenten
Versuchsvorschrift
Into a 2-L three-necked flask equipped with a gas blowing tube, a reflux condenser and a stirrer, were charged 269.7 g (2 mol) of 3,5-dimehtylbenzaldehyde and 800 g of o-dichlorobenzene. The temperature of the reaction system was controlled to 5° C. while introducing a nitrogen gas. After bubbling the reaction solution by blowing a nitrogen gas for one hour, the feed of nitrogen was stopped and the feed of chlorine was started. Simultaneously with the feed of chlorine, the irradiation of light from a mercury lamp was started. The photochlorination was completed after 6 h. The quantitative analysis by gas chromatography showed the production of 1.4 mol of 3,5-dimethylbenzoyl chloride (yield: 70%). By vacuum distillation, 236 g (1.4 mol) of 3,5-dimethylbenzoyl chloride was isolated (yield: 68%). The results of total elements analysis by ICP showed that a total content of residual group 3 to group 12 metals was 500 ppm or lower in which the highest was 10 ppm of Fe and the second highest was 30 ppm of Zn.
Aufarbeitung
- customInto a 2-L three-necked flask equipped with a gas
- customwas controlled to 5° C.
- additionwhile introducing a nitrogen gas
- customAfter bubbling the reaction solution
- customfor one hour
- customSimultaneously with the feed of chlorine, the irradiation of light from a mercury lamp
Quellen und Nachweise
- ORD-Eintrag
- ord-1ffb6230642e40d6ac635d92eca203e1
- Quelldatensatz
- uspto-grants-2008_07
- Patentnummer
- US07405331B2
Verknüpfte Notizen
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