Electric Literature of 2265-91-0,Some common heterocyclic compound, 2265-91-0, name is 1,3-Difluoro-5-iodobenzene, molecular formula is C6H3F2I, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A mixture of 8-{[tert-butyl(dimethyl)silyl]oxy}-2-azaspiro[4.5]decan-1-one (isomer 1 ) (425 mg, 1 .50 mmol), 1,3-difluoro-5-iodobenzene (360 mg, 1 .50 mmol, CAS No 2265-91-0), copper(l) iodide (143 mg, 0.750 mmol), N,N’-dimethylethylenediamine (164 muIota, 1 .50 mmol) and potassium carbonate (435 mg, 3.15 mmol) in dioxane (26 ml) was heated to 160 for 2 h in a microwave reactor. Upon cooling, the reaction mixture was filtrated through a pad of celite, and the filtrate was concentrated and the residue was purified by flash chromatography (25 g Snap Cartrige, hexanes/ethyl acetate-gradient, 0% -> 50% ethyl acetate) to give the title compound as single isomer (575 mg).LC-MS (Method 2): Rt= 1 .79 min; MS (ESIpos): m/z = 396.3 [M+H]+1H-NMR (400 MHz, DMSO-d6): delta [ppm] = 7.50-7.41 (m, 2H), 6.98-6.91 (m, 1H), 3.94-3.88 (m, 1H), 3.72 (t, 2H), 2.00-1 .85 (m, 4H), 1 .63-1 .47 (m, 4H), 1 .28-1.20 (m, 2H), 0.85 (s, 9H), 0.01 (s, 6H)
The synthetic route of 2265-91-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BAYER PHARMA AKTIENGESELLSCHAFT; BUCHGRABER, Philipp; EIS, Knut; WAGNER, Sarah; SUeLZLE, Detlev; VON NUSSBAUM, Franz; BENDER, Eckhard; LI, Volkhart, Min-Jian; LIU, Ningshu; SIEGEL, Franziska; LIENAU, Philipp; (248 pag.)WO2018/78005; (2018); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com