関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | Benzaldehyde, 3,5-dimethyl- | HCID 34225 | — |
| 生成物 | 3,5-Dimethylbenzoyl Chloride | HCID 81088 | 70% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07405331B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-1ffb6230642e40d6ac635d92eca203e1 |
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| 出典メモ | uspto-grants-2008_07 |
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