Novel Crystalline Salts of 4-Piperidyl- and 4-Pyridylmethylamines Prepared by Catalytic Hydrogenation of 4-Pyridinecarbonitrile: Crystallographic Unit Cells Based on Powder XRD Patterns by Using the <i>DASH</i> Program Package
Structures of some hydrogenated products and intermediates, prepared by a heterogeneous Pd/C or Ru/C catalyst starting from 4-pyridinecarbonitrile (<b>4PN</b>), in water and in the presence of an acidic additive (HCl or H<sub>2</sub>SO<sub>4</sub>), were confirmed...
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| Main Authors: | , |
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| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2024-10-01
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| Series: | Crystals |
| Subjects: | |
| Online Access: | https://www.mdpi.com/2073-4352/14/11/938 |
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| Summary: | Structures of some hydrogenated products and intermediates, prepared by a heterogeneous Pd/C or Ru/C catalyst starting from 4-pyridinecarbonitrile (<b>4PN</b>), in water and in the presence of an acidic additive (HCl or H<sub>2</sub>SO<sub>4</sub>), were confirmed in various salt forms of 4-piperidylmethylamine (<b>4PIPA</b>) and 4-pyridylmethylamine (<b>4PA</b>). Crystallographic unit cell structure of the completely hydrogenated product salts <b>(4PIPA·H<sub>2</sub>SO<sub>4</sub></b> and <b>4PIPA·2HCl</b>) showed a common double-protonated <b>[4PIPA+2H]<sup>2+</sup></b> divalent cation structure, also proved by FT-IR, and that of the <b>4PA·H<sub>2</sub>SO<sub>4</sub></b> intermediate salt was also indexed and modeled by means of powder X-ray diffraction, applying the <i>DASH</i> 4.0 software package and crystal coordinates coming from former single-crystal X-ray structure determination. Formations of the anhydrous and hydrated forms of <b>4PA·0.5H<sub>2</sub>SO<sub>4</sub>·xH<sub>2</sub>O</b> (x = 0 or x = 0.5, hemisulfates) were also studied by powder XRD and FT-IR spectroscopy for comparing these crystal structures. |
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| ISSN: | 2073-4352 |