Electric Literature of 1875-88-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 1875-88-3, name is 2-(4-Chlorophenyl)ethanol, molecular formula is C8H9ClO, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
In a 1 L pressure vessel, 4-chlorophenylethanol (412.8 g, 2636 mmol) was stirred and heated to an internal temperature of -91 0C. The system was held under reduced pressure (~ – 0.98 bar) for ~2 min. Hydrogen bromide gas was gradually charged into the pressure vessel and the reaction was stirred at an internal pressure between +0.69 and +1.65 bar for 135 min. The vessel was allowed to slowly vent to a caustic scrubber and flushed with nitrogen gas for ~ 5 min. Conversion to the bromide was found to be 4.27% by HPLC. The reaction mixture was allowed to cool to ambient temperature overnight under nitrogen. The mixture was then heated once more in an oil bath set at 96 0C and the vessel was evacuated. The vessel was gradually filled with hydrogen bromide gas and stirred at an internal pressure between +1.38 and +1.65 bar for 2 h. Conversion to the bromide was found to be 92.67 % by HPLC. The reaction was held at a bath temperature of 96 0C at atmospheric pressure for 45 min. The vessel was then evacuated and slowly backfilled with hydrogen bromide gas over 15 min to +1.38 bar. After stirring for a further 2.5 h at +1.24 to +1.38 bar, the vessel was vented to the caustic scrubber and held at a bath temperature of 96 0C in closed system at atmospheric pressure. Conversion to the bromide was found to be 99.49% by HPLC with a peak area purity of 98.71%.In order to test stability and impurity formation, the pressure vessel was then evacuated and gradually back filled with hydrogen bromide gas to an internal pressure of +1.03 bar. The dark brown suspension was allowed to stir at +1.03 bar at a bath temperature of 96 0C. After 15 h the internal pressure had risen to +2.41 bar and the vessel was vented to the caustic scrubber, purged with nitrogen, and allowed to cool to ambient temperature. The peak area purity was found to be 96.06%. The reaction mixture was transferred to a seperatory funnel and allowed to separate at room temp. The upper product phase was washed with water (412 mL) in 2 portions to leave a milky beige suspension (563.4 g) with an HPLC peak area purity of 99.29%.
According to the analysis of related databases, 1875-88-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ARENA PHARMACEUTICALS, INC.; WO2009/111004; (2009); A1;,
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