With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.3663-80-7,2,3-Dihydrobenzo[b][1,4]dioxine-2-carboxylic acid,as a common compound, the synthetic route is as follows.
To a solution of 2, 3-dihydrobenzo [b] [1, 4] dioxine-2-carboxylic acid (20.0 g, 111 mmol) in DCM (200 mL) was added oxalyl dichloride (30.0 g, 238 mmol) at 0 , followed by 0.5 ml of DMF. The solution was stirred at 0 for 1 hour, and at ambient temperature for 2h, and then concentrated to dryness. The resulting oil was diluted in THF (200 mL) . Malononitrile (11.0 g, 167 mmol) was added at 0 and followed by TEA (24.6 g, 167 mmol) . The final solution was stirred at ambient temperature for 16 h. The reaction mixture was filtered through a celite pad and the filtrate was added 200 mL of H2O, extracted with EA (200mL x 3) . The combined extracts were washed with brine (200mL x 3) , dried over sodium sulfate anhydrous and concentrated to get crude product (25.5 g) as brown oil, which was used in next step directly. MS: M/e 229 (M+1)+, 3663-80-7
As the paragraph descriping shows that 3663-80-7 is playing an increasingly important role.
Reference£º
Patent; BEIGENE, LTD.; ZHANG, Guoliang; REN, Bo; WANG, Hexiang; ZHAO, Haibo; GUO, Yunhang; WANG, Zhiwei; ZHOU, Changyou; (237 pag.)WO2016/8411; (2016); A1;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem