Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 615-16-7, name is 2-Hydroxybenzimidazole, A new synthetic method of this compound is introduced below., Quality Control of 2-Hydroxybenzimidazole
An ice-cold mixture of sodium hydride (8.00 g, 60% dispersion in mineral oil, 200 mmol) and 145 (8.94g, 66.6 mmol) in DMF (250 mL) under a dry nitrogen atmosphere was allowed to gradually warm to room temperature. To the resulting mixture, iodoethane (16 ml, 200 mmol) was added and the mixture was stirred at room temperature overnight. The reaction mixture was poured into ice and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over Na2SO4 and filtered. The filtrate was concentrated under reduced pressure and the residue was taken up in hexanes and filtered. The resulting brown solid was dried under reduced pressure to give 146 (9.00 g, 71% yield). This material was used without purification. [0394] Step Two: A mixture of DMF (3.6 g, 49 mmol) and POCl3 (9.6 mL, 100 mmol) was stirred at room temperature under a dry nitrogen atmosphere for 1 hour. The flask containing this mixture was then placed in a 45 C. oil bath and 146 (7.6 g, 40 mmol) was added in small portions. The oil bath temperature was raised to 70 C. and the mixture was stirred overnight, then cooled to room temperature. The mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and brine, dried over Na2SO4 and filtered. The filtrate was concentrated under reduced pressure to give a 7:3 mixture of 147:146 (6.69 g). This material was used without purification.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Biediger, Ronald J.; Chen, Qi; Decker, E. Radford; Holland, George W.; Kassir, Jamal M.; Li, Wen; Market, Robert V.; Scott, Ian L.; Wu, Chengde; Li, Jian; US2004/63955; (2004); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem