With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4442-54-0,2,3-Dihydro-1,4-benzodioxine-6-carboxylic acid,as a common compound, the synthetic route is as follows.
To a stirred solution of 0.59 G (3.3 MMOL) of 1, 4-benzodioxane-6-carboxylic acid in CH3CN (30 mL) in A-10¡ãC methanol-ice bath is added sequentially DIEA (1.65 mL, 9.5 mmol), 3 (R)-aminoquinuclidine dihydrochloride (0.62 g, 3.11 MMOL) and HATU (1.18 G, 3.11 mmol). The mixture is stirred AT-10¡ãC for 1 h, followed by warming to rt and stirring overnight. The mixture is CONCENTRATED IN VACUO to a yellow residue. The crude product is purified by flash chromatography on SIO2. Elution with CHCI3-MEOH-NH40H (90: 9: 1) gave 634 mg (71 percent) of a light yellow solid. MS (ESI) M/E 289 [M+H]. The free base (0.2220 g) and L-MALIC acid (0.107 g) are added to 1 ml of acetonitrile in a 50 ml round bottom flask. The slurry is heated on a steam bath until the solution clarified. The solution was slow cooled at rt until precipitate begins to form. The solution is sonicated to induce more rapid crystallization. Solids are filtered by vacuum filtration. Yield was 95.6percent. Analysis calculated FOR C16H20N2O3 No. C4H6O5: C, 56.87 ; H, 6.20 ; N, 6.63. Found: C, 56.66 ; H, 6.26 ; N, 6.81.
4442-54-0, The synthetic route of 4442-54-0 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; PHARMACIA & UPJOHN COMPANY; WO2004/99202; (2004); A1;,
Benzodioxan
1,4-Benzodioxane | C8H8O2 – PubChem