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 103146-25-4 as follows. Safety of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile
A four-necked flask equipped with stirrer and thermometer was charged with 250.0 g of a solution of 25.0 g (0.073 mol) of [()-4- [4-DIMETHYLAMINO-L- (4′-FLUOROPHENYL)-L-] hydroxybutyl] -3-hydroxymethylbenzonitrile in toluene, and the temperature thereof was controlled so as to be [40C.] Then, 5.77 g (0.073 mol) of pyridine, 8.33 g (0.073 mol) of vinyl butyrate, 9.93 g (0.073 mol) of o-toluic acid, and 5.0 g of an immobilized enzyme (Novozym 435) was added into the above mixture. The reaction mixture was stirred at [40C] for 21 hours under a slight flow of nitrogen, and then stirring was stopped. The enzyme was filtrated from the reaction mixture with Kiriyama [FUNNEL,] and washed with 54.1 g of toluene. As a result, a toluene layer containing (S)-4- [4-dimethylamino-1- (4′-fluorophenyl)-1-hydroxybutyl]- 3-hydroxymethylbenzonitrile (9.7 g, 0. [028] mol, yield: 38.8%, optical purity: 97.8% ee), o-toluic acid salt was obtained. The combined toluene layer was washed three times with water (250 ml, 63 ml, 63 ml) at [60C,] and an aqueous layer containing [(S)-4- [4-DIMETHYLAMINO-L- (4′-] [FLUOROPHENYL)-L-HYDROXYBUTYL]-3-LIYDROXYMETHYLBENZONITRILE] (7.8 g, 0.0228 mol, extraction yield: 80%), o-toluic acid salt was obtained.
According to the analysis of related databases, 103146-25-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; H. LUNDBECK A/S; WO2004/14821; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts