Related Products of 910251-11-5, A common heterocyclic compound, 910251-11-5, name is Potassium trifluoro(methoxymethyl)borate, molecular formula is C2H5BF3KO, 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 pressure vial was charged with Intermediate 47 (350 mg, 0.969 mmol), potassium (methoxymethyl)trifluoroborate (295 mg, 1.94 mmol), RuPhos-Pd G2 (37.6 mg, 0.048 mmol) and cesium carbonate (947 mg, 2.91 mmol). The mixture was degassed (3x, vacuumlAr). Then dioxane (10 mL) and water (1.000 mL) were added, and the reaction mixture was degassed again. The pressure vial was capped, and the reactionmixture was stirred at 100 C for 18 h. Additional amounts of potassium (methoxymethyl)trifluoroborate (295 mg, 1.938 mmol), SPhos-Pd G2 (34.7 mg, 0.048 mmol), and cesium carbonate (947 mg, 2.91 mmol) were added. The reaction mixture was degassed (3x vacuumlAr), the pressure vial was capped, and the reaction mixture was stirred at 100 C for 18 h. Additional amount of SPhos-Pd G2 (34.7 mg, 0.048 mmol) wasadded, the reaction mixture was degassed, and was stirred at 125 C for 18 h. The reaction mixture was diluted with EtOAc, and CELITE was added. Solvent was removed under reduced pressure, and the residue was purified by flash chromatography (solid loading on CELITE) to give Intermediate 56A (61 mg, 19% yield) as an off-white solid. MS(ESI) m/z: 327.0 (M+H) ?H NMR (500MHz, DMSO-d6) oe ppm 8.44 (s, 1H), 8.09 (d, J=9.6Hz, 1H), 7.81 (d, J=9.6 Hz, 1H), 7.51 – 7.46 (m, 2H), 7.44 – 7.38 (m, 2H), 7.37 – 7.31 (m,1H), 5.28 (s, 2H), 4.94 (s, 2H), 3.83 (s, 3H), 3.32 (s, 3H).
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; BRISTOL-MYERS SQUIBB COMPANY; LADZIATA, Vladimir; GLUNZ, Peter W.; HU, Zilun; WANG, Yufeng; (0 pag.)WO2016/10950; (2016); A1;,
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