関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyromellitic dianhydride | HCID 6966 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | 3,5,5-Trimethylhexylbenzene | HCID 22269440 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 2,5-Bis(4-(3,5,5-trimethylhexyl)benzoyl)terephthalic acid | HCID 22269437 | — |
反応手順
A mixture of 694.76 grams of aluminum chloride, 270.6 grams of benzene-1,2,4,5-tetracarboxylic acid dianhydride (pyromellitic dianhydride), and 1722.0 grams of 1,2-dichloroethane was stirred at 15° C. A mixture of 507.04 grams of (3,5,5-trimethylhexyl)benzene, 173.17 grams of N,N-diisopropylethylamine and 676.4 mL of 1,2-dichloroethane was added to the reaction over a period of 3.5 hours keeping the reaction temperature between 15° C. and 20° C. The mixture was allowed to stir overnight at room temperature and then added to 1200 g of ice and 1200 mL concentrated hydrochloric acid and stirred for 3 hours. The mixture was extracted with ethyl acetate and the ethyl acetate was washed several times with water. The organic phase was dried with magnesium sulfate and stripped to give a clear thick yellow slurry. To this was added 200 mL ethyl acetate followed by 600 mL of heptane and stirred for 15 minutes. The solid was collected by filtration to give 2,5-bis(4-(3,5,5-trimethylhexyl)benzoyl)terephthalic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06974877B2 |
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| 出典データセット | uspto-grants-2005_12 |
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| ORD ID | ord-e88fd6884e6c48ffba76e3a261346b6f |
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| 出典メモ | uspto-grants-2005_12 |
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