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 72179-84-1 as follows. Quality Control of (Methylsulfamoyl)amine
Material from Example 73-Step 1 (40 mg, 0.098 mmol) was dissolved in tetrahydrofuran (5 mL) and 1,1?-carbonyldiimidazole (47.5 mg, 0.293 mmol) was added. The mixture was heated to 60 C for 1 hour, then 1,8-diazabicyclo[5.4.0]undec-7-ene (44.6 mg, 0.293 mmol) and Nmethylsulfuric diamide (32.3 mg, 0.293 mmol) were added followed by stirring at room temperature for 12 hours. The mixture was concentrated, and the residue was dissolved in CH3OH (1.3 mL) to which a couple of drops of acetic acid were added to adjust the pH to 6-7. The filtered solution was purified by preparative HPLC (0.1% CF3CO2H/H20/CH3CN) to give the titled compound (28 mg, 0.056 mmol, 57.1% yield). ?H NMR (400 MHz, DMSO-d6) ppm 11.25 (s, 1H), 7.42 -7.36 (m, 1H),7.33 – 7.08 (m, 4H), 7.06 – 6.96 (m, 2H), 6.86 (d, J = 7.6 Hz, 2H), 3.73 (s, 2H), 3.26 – 3.16 (m, 3H),2.46 (s, 2H), 2.32 – 2.20 (m, 2H), 2.09 (t, J = 7.2 Hz, 1H), 1.73 (s, OH), 1.43 (s, 2H), 1.34 (s, 1H), 1.30- 1.21 (m, 1H), 1.18 (s, 1H), 1.13 (s, 1H), 1.07 (s, 1H), 0.93 (s, 1H).
According to the analysis of related databases, 72179-84-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ABBVIE INC.; BLACK, Lawrence, A.; BUNNELLE, William, H.; CHEN, Da; CLAPHAM, Bruce; DEGOEY, David, A.; DENG, Xiangjun; FU, Liqiang; HAZELWOOD, Lisa, A.; KONG, Linglong; LANG, Qingyu; LEE, Chih-Hung; LI, Mingfeng; LUNDGAARD, Greta, L.; PATEL, Meena, V.; TAO, Ruihong; ZHANG, Lin; ZHANG, Qingwei; ZHENG, Qiangang; ZHU, Wei; (289 pag.)WO2017/177004; (2017); A1;,
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