达罗他胺中间体合成中杂质的发现和结构表征

马卉芳,童悦,王荣繁,谢建伟

Discovery and Structural Characterization of Impurities in the Synthesis of Darolutamide Intermediate

MA Huifang,TONG Yue,WANG Rongfan,XIE Jianwei

表3 杂质C的NMR数据归属

Table 3 NMR assignments of impurity C

No.	¹H NMR	¹³C NMR	HMBC(¹H→¹³C)	¹H-¹H COSY
No.	δ_H	δ_C	HMBC(¹H→¹³C)	¹H-¹H COSY
1	N/A	116.3	N/A	N/A
2	N/A	111.6	N/A	N/A
3	N/A	137.1	N/A	N/A
4	8.01 (1H, d, J=1.4 Hz)	126.7	C-2, 3, 6, 8	N/A
5	N/A	139.3	N/A	N/A
6	7.81 (1H, dd, J=8.1, 1.5 Hz)	124.1	C-2, 4, 8	H-7
7	7.68 (1H, d, J=8.1 Hz)	134.1	C-1, 3, 5	H-6
8	N/A	148.5	N/A	N/A
9	6.67 (1H, d, J=2.5 Hz)	104.2	C-8, 10	H-10
10	7.70 (1H, d, J=2.5 Hz)	129.7	C-8, 9	H-9
11	5.45 (1H, dd, J=9.6, 2.6 Hz)	88.0	C-10, 12, 13, 15	H-12
12	2.13 (1H, m), 2.19 (1H, m)	30.6	C-11, 13, 14	H-11, 13
13	1.75 (1H, overlap), 2.09 (1H, m)	22.3	C-11, 12, 14, 15	H-12, 14
14	1.67 (1H, m), 1.75 (1H, overlap)	24.9	C-12, 13, 15	H-13, 15
15	3.76 (1H, m), 4.11 (1H, m)	68.0	C-11, 13, 14	H-14