X-Ray Absolute Structure of Nicergoline (Form I). Quantitative Analysis of Nicergoline Phase Mixture: Form I/Form II

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Title:X-Ray Absolute Structure of Nicergoline (Form I). Quantitative Analysis of Nicergoline Phase Mixture: Form I/Form II
Creators:
Hušák, Michal
Had, Jiří
Kratochvíl, Bohumil
Cvak, Ladislav
Stuchlík, Josef
Jegorov, Alexandr
Journal or Publication Title:
Collection of Czechoslovak Chemical Communications, 59, 7, pp. 1624-1636

Abstract

<p>The structure of semisynthetic ergot derivative nicergoline (form <i>I</i>) was determined from X-ray single crystal diffraction data. The title alkaloid (10α-methoxy-1,6-dimethylergoline-8β-methanol-5'-bromonicotinate, C<sub>24</sub>H<sub>26</sub>BrN<sub>3</sub>O<sub>3</sub>) crystallizes in the triclinic space group <i>P1</i>, with <i>a</i> = 7.729(7), <i>b</i> = 8.695(4), <i>c</i> = 17.030(8) Å, α = 100.90(4), β = 98.67(5), γ = 93.04(5)°, <i>Z</i> = 2. A structural comparison of nicergoline forms <i>I</i> and <i>II</i> was made. The quantitative analyses of some model phase mixtures form <i>I</i> / form <i>II</i> were carried out using both Rietveld full profile fitting method and linear regression of the peak intensity concentration dependence. Results obtained are in good mutual agreement. The smallest limit of detection of form <i>II</i> in binary mixture with form <i>I</i> is about 3% as found from powder diffraction study.

Title:X-Ray Absolute Structure of Nicergoline (Form I). Quantitative Analysis of Nicergoline Phase Mixture: Form I/Form II
Creators:
Hušák, Michal
Had, Jiří
Kratochvíl, Bohumil
Cvak, Ladislav
Stuchlík, Josef
Jegorov, Alexandr
Divisions:Life and Chemical Sciences > Institute of Organic Chemistry and Biochemistry > Collection of Czechoslovak Chemical Communications
Journal or Publication Title:Collection of Czechoslovak Chemical Communications
Volume:59
Number:7
Page Range:pp. 1624-1636
ISSN:0010-0765
E-ISSN:1212-6950
Publisher:Institute of Organic Chemistry and Biochemistry
Related URLs:
URLURL Type
http://dx.doi.org/10.1135/cccc19941624UNSPECIFIED
ID Code:585
Item Type:Article
Deposited On:06 Feb 2009 17:02
Last Modified:06 Feb 2009 16:02

Citation

Hušák, Michal; Had, Jiří; Kratochvíl, Bohumil; Cvak, Ladislav; Stuchlík, Josef; Jegorov, Alexandr (1994) X-Ray Absolute Structure of Nicergoline (Form I). Quantitative Analysis of Nicergoline Phase Mixture: Form I/Form II. Collection of Czechoslovak Chemical Communications, 59 (7). pp. 1624-1636. ISSN 0010-0765

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