892242-64-7, 4-((3-(4-Cyclohexylpiperazin-1-yl)-6-oxo-6H-anthra[1,9-cd]isoxazol-5-yl)amino)benzoic acid is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
892242-64-7, About 21kg of 4-((3-(4-cyclohexylpiperazin-l-yl)-6-oxo-6H-anthra[l,9- cd]isoxazol-5-yl)amino)benzoic acid was slurred in 625L of 0.4 M NaOH in MeOH and purified water (4: 1) solution under about 40-45C for about 2-4 hours. Then slowly cooled the reaction to room temperature and stirred for another 2-4 hours. After confirmed the reaction completion by HPLC, the solid was centrifuged and washed with about 57L of MTBE. The wet cake was re- suspended in about 245L of 0.1M NaOH in MeOH/H20 solution under room temperature. The wet cake was centrifuged and washed with about 56L of MTBE again. The filtered solid was re- suspended in about 250L of MTBE under room temperature for about 1-2 hours. The solid was separated and dried at 25-30C under reduced pressure for 12-24 hours to obtain the final product with purity more than 99.9% (HPLC) and about 90% yield. Mass spectra give [M+l] = 523.2. 1H-NMR (400 MHz, DMSO-d6, see Figure 1), ppm (delta): 11.79 (IH, s), 8.48 (IH, d), 8.20 (IH, d), 7.93 (2H, d), 7.84 (IH, t), 7.72 (IH, t), 7.35 (2H, d), 6.39 (IH, s), 3.85 (4H, m), 2.72- 2.70 (4H, m), 2.28-2.265 (IH, m), 1.72-1.78 (4H, m), 1.55-1.58 (IH, m), 1.08-1.23 (5H, m). Sodium content: 3.8%. The Raman spectrum is shown in Figure 4, and the XRPD data is given in Table 1 below and Figure 2, IR spectra is given in Figure 5 and DSC spectra is given in Figure 3. These data confirm the stable crystalline polymorphic form (Form A) of the compound of Formula I.
The synthetic route of 892242-64-7 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; PURDUE PHARMA L.P.; WU, Jay Jie-Qiang; WANG, Ling; (31 pag.)WO2017/27465; (2017); A1;,
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