Synthesis
B. The reaction solution from step A was transferred to a 2L four-necked flask and 60.0 g of sodium hydroxide solid was added and stirred thoroughly until completely dissolved. Subsequently, the reaction mixture was slowly heated to 60-65°C and maintained at this temperature for about 3 hours. The reaction progress was monitored by gas chromatography (GC), and after confirming that the reaction endpoint was reached, the reaction solution was cooled to 20 °C. After standing and layering, the aqueous phase was separated and slowly added to 190.1 g of 30% aqueous hydrochloric acid and the pH was adjusted to about 3.0. The organic phase was collected by standing and layering again. The organic phase was dried over anhydrous sodium sulfate to give 143.2 g of the target product 3-(3-chlorophenyl)propionic acid in 77.6% yield.
