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2 化合物3的NMR数据归属

Table 2 NMR assignments of compound 3

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	115.7	N/A	N/A
2	N/A	113.0	N/A	N/A
3	N/A	137.2	N/A	N/A
4	7.79 (1H, d, J=1.4 Hz)	130.2	C-2, 6, 8	N/A
5	N/A	136.2	N/A	N/A
6	7.59 (1H, dd, J=8.0, 1.5 Hz)	127.4	C-2, 3, 4, 7, 8	H-7
7	7.78 (1H, d, J=8.1 Hz)	134.1	C-1, 3, 5	H-6
8	N/A	141.1	N/A	N/A
9	6.46 (1H, d, J=1.8 Hz)	108.0	C-5, 8, 10, 11	H-10
10	7.64 (1H, d, J=1.6 Hz)	139.7	C-8, 9	H-9
11	5.15 (1H, dd, J=10.0, 2.4 Hz)	84.6	C-8, 12, 13, 15	H-12
12	1.90 (1H, m), 2.59 (1H, m)	29.5	C-11, 13, 14	H-11, 13
13	1.62 (1H, overlap), 2.12 (1H, m)	22.8	C-11, 12, 14, 15	H-12, 14
14	1.62 (1H, overlap), 1.78 (1H, m)	24.8	C-12, 13, 15	H-13, 15
15	3.64 (1H, m), 4.17 (1H, m)	67.6	C-11, 13, 14	H-14