With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.132710-90-8,1-Boc-4-(3-hydroxypropyl)piperazine,as a common compound, the synthetic route is as follows.
Triphenylphosphine (2.059 g, 7.85 mmol), tett-butyl 4-(3-hydroxypropyl)piperazine-1-carboxylate (1.692 g, 6.93 mmcl) and diisopropyl (E)-diazene-1,2-dicarboxylate (1.587 g, 7.85mmcl) were mixed in THE (20 mL) at 0 C, and then 4-chloro-3-hydroxy-5-nitrobenzamide (1 g, 4.62 mmcl) was added. The reaction solution was maintained at RT for 16 hrs then the brown reaction solution was partitioned between sat. NaHCO3 (aq) and EtOAc. The organic layer was washed with brine, dried over Mg504, concentrated and purified on silica gel (20 %80 % (3:1 EtOAc/EtOH) I Hexane, with 2% NH4OH; 330 g RediSep column). Desired fractions were combined and concentrated to give the title compound as a white solid (970 mg, 47 % yield). 1H NMR (400 MHz, DMSO-d6) ppm 8.30 (s, 1 H), 8.05 (d, J=1.77 Hz, 1 H), 7.88 (d, J=1.77 Hz, 1 H), 7.80 (s, 1 H), 4.28 (t, J=6.21 Hz, 2 H), 3.31 (br. s., 4 H), 2.48 (t, J=7.10 Hz, 2 H), 2.33 Ct, J=4.94 Hz, 4 H), 1.96 Ct, J=6.59 Hz, 2 H), 1.40 Cs, 9 H). LCMS CLCMS Method K):Rt = 0.69 mm, [M+H] = 443.4.
132710-90-8, 132710-90-8 1-Boc-4-(3-hydroxypropyl)piperazine 16217800, apiperazines compound, is more and more widely used in various fields.
Reference：
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; CHARNLEY, Adam Kenneth; DARCY, Michael Gerard; DODSON, Jason W.; DONG, Xiaoyang; FAVRE, David; HUGHES, Terry Vincent; KANG, Jianxing; LEISTER, Lara Kathryn; LI, Yuehu; LIAN, Yiqian; MEHLMANN, John F.; NEVINS, Neysa; RAMANJULU, Joshi M.; ROMANO, Joseph J.; WANG, Gren Z.; YE, Guosen; ZHANG, Daohua; (489 pag.)WO2019/69269; (2019); A1;,
Piperazine – Wikipedia
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