Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (4): 430-436.DOI: 10.3724/SP.J.1123.2020.10013
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WANG Yiyun1,2, LÜ Xiaofang1, XU Haojie1,2, MENG Zihu1,*(), LI Jiarong1, XU Zhibin1, XUE Min1
Received:
2020-10-28
Online:
2021-04-08
Published:
2021-03-08
Contact:
MENG Zihu
CLC Number:
WANG Yiyun, LÜ Xiaofang, XU Haojie, MENG Zihu, LI Jiarong, XU Zhibin, XUE Min. Separation and identification of impurities from intermediates of istradefylline[J]. Chinese Journal of Chromatography, 2021, 39(4): 430-436.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.10013
Fig. 4 HPLC chromatogram of intermediate A1 and its relative substances Column: Agilent Zorbax C18 column (150 mm×4.6 mm, 5 μm); column temperature: 35 ℃; mobile phase: acetonitrile (A) and water (B); flow rate: 1.0 mL/min; gradient elution (tmin/A: B)=t0/20:80, t15/60:40, t20-t50/90:10; detection wavelength: 268 nm.
Structure | ||||
No. of C | δC/δH | HSQC | HMBC | C |
1 | 153.3 | - | H-7, 5 | 4° |
2 | 152.2 | - | H-5 | 4° |
3 | 81.9/5.85 | H-3 | - | 3° |
4 | 162.0 | - | H-7 | 4° |
5 | 34.9/3.74 | H-5 | H-6 | 2° |
6 | 13.9/1.02 | H-6 | H-5 | 1° |
7 | 36.9/3.94 | H-7 | H-8 | 2° |
8 | 14.1/1.07 | H-8 | H-7 | 1° |
9 | 159.3 | - | H-10 | 4° |
10 | 34.6/3.04 | H-10 | H-11 | 2° |
11 | 15.9/1.01 | H-11 | H-10 | 1° |
Table 1 HSQC and HMBC NMR data of the impurity
Structure | ||||
No. of C | δC/δH | HSQC | HMBC | C |
1 | 153.3 | - | H-7, 5 | 4° |
2 | 152.2 | - | H-5 | 4° |
3 | 81.9/5.85 | H-3 | - | 3° |
4 | 162.0 | - | H-7 | 4° |
5 | 34.9/3.74 | H-5 | H-6 | 2° |
6 | 13.9/1.02 | H-6 | H-5 | 1° |
7 | 36.9/3.94 | H-7 | H-8 | 2° |
8 | 14.1/1.07 | H-8 | H-7 | 1° |
9 | 159.3 | - | H-10 | 4° |
10 | 34.6/3.04 | H-10 | H-11 | 2° |
11 | 15.9/1.01 | H-11 | H-10 | 1° |
Parameter | Content |
---|---|
Empirical formula | C11H18N4O3 |
Formula weight | 254.29 |
Temperature/K | 296(2) |
Crystal system | monoclinic |
Space group | P21/n |
a/nm | 0.5076(3) |
b/nm | 1.8133(10) |
c/nm | 1.3835(8) |
α/° | 90 |
β/° | 95.670(9) |
γ/° | 90 |
Volume/nm3 | 1.267(12) |
Z | 4 |
Reflections collected | 11865 |
Final R indices [I>=2σ (I)] | R1=0.0623, wR2=0.1617 |
Final R indices [all data] | R1=0.1589, wR2=0.2145 |
Table 2 Crystal data for the impurity
Parameter | Content |
---|---|
Empirical formula | C11H18N4O3 |
Formula weight | 254.29 |
Temperature/K | 296(2) |
Crystal system | monoclinic |
Space group | P21/n |
a/nm | 0.5076(3) |
b/nm | 1.8133(10) |
c/nm | 1.3835(8) |
α/° | 90 |
β/° | 95.670(9) |
γ/° | 90 |
Volume/nm3 | 1.267(12) |
Z | 4 |
Reflections collected | 11865 |
Final R indices [I>=2σ (I)] | R1=0.0623, wR2=0.1617 |
Final R indices [all data] | R1=0.1589, wR2=0.2145 |
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