Related Products of 15862-50-7, 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 15862-50-7 as follows.
Dioxane (10.4 L, 8 v), 1 (1.3 kg, 1.0 eq.), KOAc (1.65 kg, 3.0 eq.), and B2Pin2 (1.7 kg, 1.2 eq.) were charged into 20 L reactor. Nitrogen was bubbled into the solution to remove any excess oxygen for 1 hour at 20~30C. Pd(dppf)Cl2 (125.6 g, 0.03 eq.) was into the reactor into the mixture under nitrogen. The mixture was heated to 80~90C. Thehe reaction mixture stirred for 3 hours at until HPLC showed the reaction was completed. The reaction mixtiire was cooled to 20-30C and then filtered. The filtered cake was washed with dioxane (2.6 L, 2 v). The filtered solutions were combined and concentrated and then transferred to 20 L reactor. H2O2 (3.25 L, 2.5 v) was added at 20~50C, and the temperature was increased from 23 to 50C. The reaction misture was stirred for 30-60 min until HPLC showed the reaction was completed. H2O (6.5 L, 5 v) was added in to the mixture, and the mixture was extracted with DCM (13.0 L, 10 v) twice. The organic phase was collected and washed with 15% brine (6.5 L, 5 v) twice, and was then extracted with 15% Na2C03 (6.5 L, 5 L) twice. The aqueous phase was colleted and the pH value was ajdjusted 10-1 1 to 4-5 with 3M HC1. The aqueous phase was then extracted with EA (13.0 L, 10.0 v) twice. The organic phase was collected and concentrated to about dryness, and heptane (6.5 L, 5.0 v) was added to slurry for 1 hour at 20~30C. The slurry was filtered, and the filtered cake was washed with heptane (650 ml, 0.5 v), drid in oven at 30~40C for overnight to obtain 650.2 g product as brown solid with purity: 99.6%, yield: 67.8%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,15862-50-7, its application will become more common.
Reference:
Patent; EPIZYME, INC.; CAMPBELL, John Emmerson; DUNCAN, Kenneth William; MILLS, James Edward John; MUNCHHOF, Michael John; (301 pag.)WO2019/79540; (2019); A1;,
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