1215205-50-7, name is Ethyl 1-(4-bromophenyl)cyclopropanecarboxylate, belongs to esters-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C12H13BrO2
Example 30 1-(1-{4-[1-(Ethoxycarbonyl)cyclopropyl]benzoyl}piperidin-4-yl)-3-methylpiperidine trifluoroacetic acid salt 600 mg (2.2 mmol) of ethyl 1-(4-bromophenyl)cyclopropanecarboxylate, 813 mg (4.5 mmol) of 4-(3-methylpiperidin-1-yl)piperidine, 294 mg (1.12 mmol) of molybdenum hexacarbonyl, 105 mg (0.11 mmol) of trans-bis(acetate)bis[o-(di-o-tolylphosphine)benzyl]dipalladium(II) (Herrmann’s palladacycle) and 709 mg (6.7 mmol) of sodium carbonate were suspended in 3 ml of water and heated in a microwave at 150 C. for 10 minutes. After cooling, the mixture was extracted with ethyl acetate and then filtered. The organic phase was removed from the filtrate, dried over magnesium sulphate and filtered, and the filtrate was concentrated. The residue was purified by preparative HPLC. [Reprosil C18, 10 mum, 250 mm*30 mm (50% methanol/50% water (+0.05% trifluoroacetic acid) to 70% methanol/30% water (+0.05% trifluoroacetic acid)) over a run time of 25 min]. The product-containing fractions were combined, concentrated and dried under HV. This gave 348 mg (30% of theory) of an oil. LC-MS [Method 2]: Rt=0.74 min; MS (ESIpos): m/z=399 (M-CF3COOH+H)+ 1H-NMR (400 MHz, DMSO-d6): delta [ppm]=0.88-0.94 (m, 3H), 1.11 (t, 3H), 1.20-1.26 (m, 2H), 1.49-1.55 (m, 2H), 1.59-2.19 (m, 8H), 2.58-3.14 (m, 5H), 3.33-3.55 (m, 3H), 3.58-3.88 (m, 1H), 4.04 (q, 2H), 4.29-4.81 (m, 1H), 7.32-7.38 (m, 2H), 7.39-7.43 (m, 2H), 8.98-9.38 (m, 1H)
The synthetic route of 1215205-50-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Bayer Pharma Aktiengesellschaft; BECKER-PELSTER, Eva Maria; BUCHGRABER, Philipp; BUCHMUeLLER, Anja; ENGEL, Karen; GNOTH, Mark Jean; HIMMEL, Herbert; KAST, Raimund; KELDENICH, Joerg; KLAR, Juergen; KNORR, Andreas; LANG, Dieter; LINDNER, Niels; SCHMECK, Carsten; SCHOHE-LOOP, Rudolf; TINEL, Hanna; TRUeBEL, Hubert; WUNDER, Frank; (97 pag.)US2016/318866; (2016); A1;,
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