Structural studies on lithocholyl-N-(2-aminoethyl)amide in the solid state

被引：7

作者：

Ahonen, Kari ^{[1
]}

Behera, Babita ^{[1
]}

Sievanen, Elina ^{[1
]}

Valkonen, Arto ^{[1
]}

Lahtinen, Manu ^{[1
]}

Tolonen, Minna ^{[1
]}

Kauppinen, Reijo ^{[1
]}

Kolehmainen, Erkki ^{[1
]}

机构：

[1] Univ Jyvaskyla, Dept Chem, Jyvaskyla 40014, Finland

来源：

STRUCTURAL CHEMISTRY | 2010年 / 21卷 / 01期

关键词：

C-13 and N-15 CP/MAS; PXRD; Polymorph; Solvate; Lithocholyl amide; GRAM-NEGATIVE BACTERIA; BILE-ACID DERIVATIVES; SUPRAMOLECULAR CHIRALITY; POWDER DIFFRACTION; CRYSTAL-STRUCTURE; NMR-SPECTROSCOPY; CINNAMIC ACID; CPMAS NMR; POLYMORPHISM; C-13;

D O I：

10.1007/s11224-009-9560-7

中图分类号：

O6 [化学];

学科分类号：

0703 ;

摘要：

The synthetic procedure of lithocholyl-N-(2-aminoethyl)amide yielded a mixture of several forms detected by solid state C-13 CP/MAS NMR although the solution state NMR unambiguously ascertained that the compound was pure. By recrystallization from various solvents one pure polymorph alongside with four solvates were isolated. The structures of the pure polymorph and the solvates were characterized by C-13 and N-15 CP/MAS NMR and powder X-ray diffraction (PXRD) methods. Variable contact time and dipolar dephasing experiments were employed to obtain optimized CP parameters and to distinguish various CH (n) (n = 0-3) resonances. CSA analyses of spinning side bands at different spinning rates showed small variations in the shielding tensor values of the carbonyl group between the pure polymorph (recrystallized from acetonitrile, tetrahydrofuran and 1,4-dioxane) and p-xylene solvate.

引用

页码：185 / 190

页数：6

共 44 条

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