Reference of 252881-74-6, 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 252881-74-6 as follows.
SI- 16 (202 mg, 0.69 mmol, 1.2 eq.), COMU (296 mg, 0.69 mmol, 1.2 eq.), and N- methylmorpholine (190 pL, 1.7 mmol, 3 eq.) were dissolved in 1.5 mL DMF and incubated for 1 min. Amino-PEG3-t-butyl ester (160 mg, 0.58 mmol, 1 eq.) was added in 2.5 mL DMF and the reaction was stirred for 2h. The reaction was diluted with ethyl acetate (15 mL) and acidified with 1N HC1 to pH 3. The organic layer was washed with water (3x 25 mL) and brine (25 mL), dried over anhydrous MgS04, and concentrated under reduced pressure. The resulting residue was purified by flash chromatography to provide the title compound as a colorless oil (215 mg, 57%). NMR (500 MHz, Chloroform-if) d 7.66 (d, j= 8.7 Hz, 2H), 7.33 (d, j= 8.7 Hz, 2H), 6.97 (dd, J= 8.8, 7.2 Hz, 4H), 6.82 (d, J= 5.4 Hz, 1H), 3.63 (t, J= 6.5 Hz, 2H), 3.62 – 3.57 (m, 10H), 3.54 (td, J= 4.8, 4.4, 1.1 Hz, 2H), 2.43 (t, J= 6.5 Hz, 2H), 1.39 (s, 9H). HRMS (ESI) [M+H]+ for CieHseBrNiOe 551.1751, found 551.1751.
According to the analysis of related databases, 252881-74-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; THE SCRIPPS RESEARCH INSTITUTE; ZHANG, Xiaoyu; CROWLEY, Vincent; CRAVATT, Benjamin; (121 pag.)WO2020/77278; (2020); A1;,
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