103146-25-4, A common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, molecular formula is C20H23FN2O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
19.5 g (115.7 mmol) of 48% hydrobromic acid was added dropwise to the solution at 30 C. or lower over 30 minutes. At about 25 C., 60.0 mg (0.18 mmol) of hydrobromide of diol compound (4) was added as a seed crystal and stirred for 30 minutes to confirm crystallization of hydrobromide of diol compound (4). did. Then, it was cooled to around 5 C., and 48.6 g (288.5 mmol) of 48% hydrobromic acid was added dropwise at around 5 C. over 30 minutes. After stirring for 1 hour at around 5 C., the precipitated crystals were separated by centrifugation and washed with 100 mL of water. Further, the crystals were washed with 100 mL of ethyl acetate. The obtained wet body is dried at 40 C. for 15 hours and then dried.118.4 g (279.8 mmol) of hydrobromide of the compound (4) was obtained. The isolated yield of the hydrobromide salt of the diol compound (4) was 97.0% based on the number of moles of the diol compound (4). Moreover, as a result of measuring the obtained hydrobromide salt of the diol compound (4) by HPLC, the purity of the hydrobromide salt of the diol compound (4) was 99.54%. Further, during crystallization of the hydrobromide salt of the diol compound (4), no crystal adhesion (scaling) was observed on the container wall surface.
The synthetic route of 103146-25-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tokuyama Corporation; Miyanoku, Takayuki; Yokoo, Yoshihiro; (12 pag.)JP2019/119710; (2019); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts