934-98-5, 2-(4-Methylpiperazin-1-yl)ethanamine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
A 250 mL round bottom flask equipped with a stir bar was charged with Example 1U (1.96 g) and anhydrous dichloromethane (160 mL) at room temperature under nitrogen. The mixture was cooled to 0¡ã C. in an ice bath, and 2-(4-methylpiperazin-1-yl)ethanamine (0.395 mL) was added via a syringe. The mixture was stirred for 25 minutes at 0¡ã C., and sodium triacetoxyborohydride (156 mg) was added as a solid. The reaction mixture was stirred for 15 minutes at 0¡ã C., and powdered activated 3 angstrom molecular sieves were added (1.96 g). The reaction mixture was stirred 2 hours at 0¡ã C., and was allowed to stir and warm slowly to room temperature overnight. LC/MS indicated one major peak with a mass that corresponded to desired product. The reaction mixture was quenched with dichloromethane and water. The layers were separated, and aqueous layer was extracted with dichloromethane and 10percent methanol/dichloromethane. The aqueous layer was neutralized with saturated aqueous NaHCO3 mixture, and was extracted one more time with 10percent methanol/dichloromethane. The combined extracts were washed with saturated aqueous NaHCO3 and brine, dried with Na2SO4, filtered, and concentrated. The residue was dissolved in dichloromethane and was purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 750 g silica gel column eluting with a gradient of 0-20percent of methanol/dichloromethane over 40 minutes. The mixed fractions were purified on a Grace Reveleris X2 MPLC using a Teledyne Isco RediSep? Rf gold 330 g silica gel column eluting with a ramp of 0-15percent of methanol/dichloromethane over 40 minutes to collect additional title compound. The material from both columns was combined to provide the title compound. 1H NMR (501 MHz, dimethyl sulfoxide-d6) delta ppm 8.61 (m, 2H), 7.47 (m, 2H), 7.39 (d, 1H), 7.17 (m, 7H), 7.04 (td, 1H), 6.96 (dd, 1H), 6.67 (d, 1H), 6.51 (d, 1H), 5.84 (dd, 1H), 5.06 (m, 2H), 4.07 (ddq, 2H), 3.90 (d, 1H), 3.75 (s, 3H), 3.68 (dd, 2H), 3.50 (d, 1H), 3.17 (m, 1H), 3.08 (m, 1H), 2.90 (m, 2H), 2.65-2.20 (m, 10H), 2.14 (s, 3H), 1.67 (s, 3H), 1.09 (t, 3H). MS (ESI) m/z 928.4 (M+H)+., 934-98-5
The synthetic route of 934-98-5 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; AbbVie Inc.; AbbVie Deutschland GmbH & Co. KG; Brady, Patrick B.; Braje, Wilfried; Dai, Yujia; Doherty, George A.; Gong, Jane; Jantos, Katja; Ji, Cheng; Judd, Andrew S.; Kunzer, Aaron R.; Lai, Chunqiu; Mastracchio, Anthony; Risi, Roberto M.; Song, Xiaohong; Souers, Andrew J.; Sullivan, Gerard M.; Tao, Zhi-Fu; Teske, Jesse A.; Wang, Xilu; Wendt, Michael D.; Yu, Yiyun; Zhu, Guidong; Penning, Thomas D.; (218 pag.)US2019/55264; (2019); A1;,
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