New learning discoveries about 3,5-Dimethoxybenzonitrile

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 19179-31-8, and friends who are interested can also refer to it.

19179-31-8, 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 19179-31-8 as follows.

Synthesis of Intermediate (1)(1 )Molecular Weight: 163.17 Molecular Weight: 197.3[00378] In a 3-neck 100 mL round-bottomed flask, 3,5-dimethoxy benzonitrile (10.0 g, 1 eq.), NaSH H20 (9.43 g, 2.0 eq.) and MgCl26H20 (12.43 g, 1.0 eq.) were dissolved in DMF (100 mL, 10 Vol.). The reaction mixture was stirred at room temperature for 2 h. Reaction completion was monitored on TLC using ethyl acetate: n-hexane (2:8)as mobile phase. Reaction mixture was brought to room temperature and quenched into the ice-water slurry (100 mL) and compound was extracted in the ethyl acetate (50 mL x 3). Organic layer was washed with brine solution (50 mL x 3) followed by drying using anhydrous sodium sulphate. Organic layer was concentrated under reduced pressure to afford 2.5 g of crude compound, yield (20.68 %). Mass/LCMS: 197.0 NMR: Confirmed.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 19179-31-8, and friends who are interested can also refer to it.

Reference:
Patent; KARYOPHARM THERAPEUTICS, INC.; SHECHTER, Sharon; KAUFFMAN, Michael; SANDANYAKA, Vincent, P.; SHACHAM, Sharon; WO2011/109799; (2011); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts