Application of 56987-35-0, These common heterocyclic compound, 56987-35-0, name is 3,3-Dibromo-azepan-2-one, its 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 solution of 3,3-dibromoazepan-2-one (15.7 g, 57.9 mmol) in piperidine (140 mL) was heated at reflux for 4.5 h under N2. The solution was then allowed to reach room temperature and washed with 0.50 M aq. NaHS03 (200 mL). The aqueous phase was extracted with CHC13 (3 x 100 mL) and the combined organic layers were washed with brine (1 x 300 mL), dried (MgS04) and concentrated to afford a brown, oily solid, that crystallized upon standing. The resulting solid was suspended in water, filtered, and washed with water and Et20 to give 1 (10.3 g, 91%) as a white solid: IR (ATR, neat) 3193, 2950, 2935, 2923, 2855, 1655, 1605 cm”1; 1H NMR (CDC13, 600 MHz) delta 6.51 (bs, 1 H), 5.06 (t, 1 H, J= 7.6 Hz), 3.22 (q, 2 H, J= 6.5 Hz), 2.78 (app t, 4 H, J= 5.3 Hz), 2.15 (q, 2 H, J= 7.2 Hz), 1.76 (app quint, 2 H, J= 6.8 Hz), 1.69-1.62 (m, 4 H), 1.54-1.48 (m, 2 H); 13C NMR (CDC13, 150 MHz) delta 171.5, 147.6, 105.4, 50.1, 39.5, 30.2, 25.5, 24.5, 21.5; HRMS (EI) m/z calcd for CiiH18N20 194.1419, found 194.1422.
Statistics shows that 3,3-Dibromo-azepan-2-one is playing an increasingly important role. we look forward to future research findings about 56987-35-0.
Reference:
Patent; UNIVERSITY OF PITTSBURGH – OF THE COMMONWEALTH SYSTEM OF HIGHER EDUCATION; WIPF, Peter; WANG, Qiming, Jan; WO2012/78859; (2012); A2;,
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