Reference of 755027-18-0, 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 755027-18-0 as follows.
in a sealable reaction tube was added i-brorno-4-iodo-2-rnethoxybenzene (2461 mg, 7.86 mrnol). tert-butyl I -oxo-2.8-diazaspiro[4.5] decane-8-carboxyiate (1000 mg, 3.93 mrnol), cesium carbonate (2562 mg, 7.86 rnrnol) and dioxane (7864 il). The reaction was purged with nitrogen. Then 9,9-dimethyi-4,5- bis(diphenyiphosphino)xanihene (341 rng, 0.590 mmol), Pd2(dba)3 (180 rng, 0.197 mrnoi)was added and nitrogen was bubbled through reaction for I mm. The reaction wassealed and stirred at 100 C overnight. The reaction was partitioned between EtOAc(50 ml) and water (30 ml). The organic layer was separated, washed with water (2 x 30m1) and brine (30 ml). dried over MgSO4, filtered and concentrated. The residue was purified using ISCO system (0-100% EtOAc/Hex gradient) to give tert-butyl 2-(4-bromo-3- rnethoxvphenyi)-i-oxo-2,8-diazaspiro[45]decane-8-carboxyiate (1.6 g, 364 mrnoi, 93 %yield) as a beige solid. ?H NMR (500MHz, DM50-do) d 7.67 (d, .J=2.2 Hz, 1H), 755(d, J=8.5 Hz, IH), 7.12 (dd, J=8.8, 2.5 Hz, 1H), 3.96 – 3.78 (m, 7H), 3.10 -2.84 (rn, 2H),2.10 (t. J=6.9 Hz, 21-1), 1.62 (dd, J=12.0, 4.0 Hz. 21-1), 1.51 (d, J=i3.5 Hz, 2F1), 1.42 (s,9H). MS (ESI) m/-: 43c.0, 441.0 (M+H).
According to the analysis of related databases, 755027-18-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHU, Yeheng; DEWNANI, Sunita, V.; EWING, William, R.; (265 pag.)WO2019/89868; (2019); A1;,
Iodide – Wikipedia,
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