In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 10297-05-9 as follows. Recommanded Product: 10297-05-9
3.98 1-(4-Chlorobutyl)-13-dihydrobenzoimidazol-2-one (56NK92) Sodium hydride (400 mg, 10 mmol, 60percent in oil) was washed with dry DMF (10 ml) under an argon atmosphere then DMF (10 ml) was added. The slurry of NaH in DMF was added slowly to 2-hydroxybenzimidazole (1.34 g, 10 mmol) in DMF (10 ml) at 0° C. under argon. The reaction was stirred at 0° C. for 20 min then 1-chloro-4-iodobutane (2.18 g, 10 mmol) in DMF (5 ml) was added slowly. The reaction was stirred at r.t. for 1.5 h then water (10 ml) was added and the reaction acidified with HCl (2M, few drops) then made basic with aqueous sodium hydrogen carbonate solution. The product was extracted with EtOAc (3*30 ml) and the organic layer was washed with aqueous sodium thiosulphate solution (10 ml), aqueous magnesium sulphate solution (4percent, 2*10 ml), brine (10 ml), dried (K2CO3), filtered and concentrated in vacuo before being purified by using an Isco CombiFlash Sq 16x [10 g silica column, eluding heptane (5 min), 0-40percent EtOAc in heptane (35 min), 40percent EtOAc in heptane (20 min)] to give the title compound (56NK92) as a pale yellow oil (416 mg, 19percent). 1H NMR (CDCl3) delta 10.48 (br. s, 1H), 7.26-7.00 (m, 4H), 3.95 (t, J=6.8 Hz, 2H), 3.59 (t, J=6.3 Hz, 2H), 1.97 (m, 2H), 1.87 (m, 2H); 13C NMR (CDCl3) delta 158.88, 130.08, 128.14, 121.56, 121.25, 109.82, 107.74, 44.32, 39.88, 29.53, 25.66; HPLC-MS (ammonium acetate) [M+H]+=225.2.
According to the analysis of related databases, 10297-05-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Kelly, Nicholas Michael; Koch, Kristian Norup; Tolf, Bo-Ragnar; US2004/67931; (2004); A1;,
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