In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 92-30-8,2-(Trifluoromethyl)-10H-phenothiazine, as follows.92-30-8
To a mixture of 2-(trifluoromethyl)-l0i7-phenothiazine (5.0 g, 18.726 mmol) and NaH (0.674 g, 28.09 mmol) in DMF (50 mL) was added 2-(bromomethyl)oxirane (3.8 g, 28.09 mmol) at 0 C. The mixture was allowed to slowly warm to rt and was stirred at room temperature overnight. Then the mixture was added to water (100 mL) and extracted with EtOAc (100 mL x 3). The combined organic layers were washed with brine (30 mL), dried over sodium sulfate, and concentrated to dryness. The residue was purified by column chromatography on silica gel (PE/EtOAc = 8/1) to afford compound 2-1 (4.5 g, 75% yield) as a white solid. ‘H NMR (400 MHz, -DMSO) S ppm 7.40-7.34 (m, 2H), 7.29-7.22 (m, 2H), 7.19-7.17 (m, 1H), 7.13- 7.18 (d, J= 7.6 Hz, 1H), 7.03-6.99 (m, 1H), 4.44 -4.40 (m, 1H), 3.83-3.78 (m, 1H), 3.28-3.24 (m, 1H), 2.89-2.87 (t, J= 4.8 Hz, 1H), 2.79-2.77 (m, 1H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. 2-(Trifluoromethyl)-10H-phenothiazine, We look forward to the emergence of more reaction modes in the future.
Reference£º
Patent; CAMP4 THERAPEUTICS CORPORATION; BUMCROT, David, A.; SEHGAL, Alfica; HERTZOG, Donald L.; (172 pag.)WO2019/195789; (2019); A1;,
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