반응식
Cl.[CH:2]([C:5]1[S:14][C:13]2[NH:12][C:11]3[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=3[N:9]=[C:8]([NH2:19])[C:7]=2[CH:6]=1)([CH3:4])[CH3:3].[CH3:20][O:21][CH2:22][CH2:23][C@H:24]1[CH2:29]N[CH2:27][CH2:26][NH:25]1>N1C=CC=CC=1>[CH3:20][O:21][CH2:22][CH2:23][C@@H:24]1[NH:25][CH2:26][CH2:27][N:19]([C:8]2[C:7]3[CH:6]=[C:5]([CH:2]([CH3:4])[CH3:3])[S:14][C:13]=3[NH:12][C:11]3[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=3[N:9]=2)[CH2:29]1참가 물질
실험 절차
Combine 2-isopropyl-4H-3-thia-4,9-diaza-benzo[f]azulene-10-ylamine hydrochloride (0.31 g, 1.04 mmol) and (S)-2-(2-methoxy-ethyl)-piperazine (0.30 g, 2.08 mmol) with anhydrous pyridine (4 mL), heat to 110° C. and stir overnight. Cool to ambient temperature to give crude material. Purification by cation exchange chromatography, eluting with solutions of 2M ammonia in methanol, in dichloromethane, (2%, 5%, 10%), and 2M ammonia in methanol, followed by flash chromatography, eluting with a gradient of solutions of 2M ammonia in methanol, in dichloromethane (2-4%), to give the title compound: mass spectrum (APCI, m/e): 385 (M+1); NMR (1H, 300 MHz, DMSO-d6),δ (ppm): 7.60 (s, 1H), 6.86-6.73 (m, 3H), 6.67 (m, 1H), 6.30 (s, 1H), 3.78 (m, 2H), 3.38-3.33 (m, 2H), 3.19 (s, 3H), 3.01-2.60 (m, 6H), 2.39 (m, 1H), 1.51 (m, 2H), 1.17 (d, 6H, J=7.5 Hz).
후처리
- customto give crude material
- customPurification by cation exchange chromatography
- washeluting with solutions of 2M ammonia in methanol, in dichloromethane, (2%, 5%, 10%)
- washeluting with a gradient of solutions of 2M ammonia in methanol, in dichloromethane (2-4%)
출처 및 근거
- ORD 기록
- ord-33a5cfe0f5d44f3190a6a729bc000608
- 출처 데이터셋
- uspto-grants-2008_06
- 특허 번호
- US07384934B2
연결된 노트
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