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. 24036-52-0, name is 6-Bromo-2H-1,4-benzoxazin-3(4H)-one, A new synthetic method of this compound is introduced below., COA of Formula: C8H6BrNO2
A mixture of 6-bromo-2H-benzo[b][1,4]oxazin-3(4H)-one (197 mg, 0.864 mmol), (S)-3-phenylmorpholine (172.7 mg, 1.058 mmol), 2-(dicylclohexylphosphino)-2′-(N,N-dimethylamino)biphenyl (11.2 mg, 0.028 mmol), tris(dibenzylideneacetone)dipalladium (0) (8.9 mg, 0.01 mmol), tetrahydrofuran (3.3 mL) and lithium bis(trimethylsilyl)amide in tetrahydrofuran (1 M, 1.93 mL, 2 mmol) was stirred at 70 C. overnight. The mixture was cooled to room temperature and saturated aqueous ammonium chloride and ethyl acetate were added. The layers were separated and the aqueous layer was extracted with ethyl acetate (3*). The organic layers were combined, dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel column chromatography (gradient: 0-25% ethyl acetate in heptanes) to afford the title compound (105.6 mg, 39.4%). 1H NMR (400 MHz, CHLOROFORM-d) delta ppm 3.01(1H, ddd, J=12.2, 9.3, 4.3 Hz), 3.29 (1H, m), 3.54 (1H, dd, J=11.4, 8.9 Hz), 3.92 (3H, m), 4.15 (1H, m), 4.48 (2H, s), 5.28 (1H, s), 6.37 (1H, d, J=2.5 Hz), 6.56 (1H, m), 6.72 (1 H, d, J=8.8 Hz), 7.16 (3H, m), 7.26 (1H, m), 7.24 (2H, s), 7.97 (1H, s).
The synthetic route of 24036-52-0 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Pfizer Inc; US2011/281854; (2011); A1;,
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