関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,4-Benzenedimethanamine | HCID 68315 | — |
| 反応物 | [1-(Aminomethyl)cyclohexyl]methanamine | HCID 71994 | — |
| 生成物 | 1,4-Dicyanobenzene | HCID 12172 | — |
反応手順
5.1 g of terephthalonitrile, 1.0 g of catalyst (Ni 5136P from Harshaw/Filtrol--contains 65% nickel on a silica-alumina support), and about 85 g of ethanol/ammonia (contains about 10 wt % ammonia) were charged to a 300 cc stainless steel pressure reactor. After a nitrogen purge, the vessel was charged to a pressure of 500 to 1000 psi with hydrogen. The temperature was then increased until the reaction temperature of 150° C. had been obtained (typically 20-30 min). After the desired reaction interval, the contents were cooled and sampled. Product analysis and conversion were determined by gas chromatography. Yields of para-xylylenediamine varied between 63-81% depending on hydrogen pressure and reaction time which is preferrably from 2 to 8 hours. The remainder of the product was saturated para-xylylenediamine (1.4 bis (aminomethyl) cyclohexane. Table IV sets forth specific examples of reactions run to obtain the diamines from hydrogenation of terephthalonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04973746 |
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| 出典データセット | uspto-grants-1990_11 |
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| ORD ID | ord-6b095c98046f4a018ffc8999ecc5e1bc |
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| 出典メモ | uspto-grants-1990_11 |
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