A method for preparing o-desvenlafaxine
A technology of desvenlafaxine and toluene, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxyl compounds, etc., can solve the problems of harsh reaction conditions, Pd residue, flammability, etc., and is beneficial to industrial production , the effect of mild reaction conditions and shortened reaction time
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Embodiment 1
[0029] Under the protection of nitrogen, add 72.0g of sodium sulfide nonahydrate and 50ml of N-methylpyrrolidone to the three-necked flask with water separator, stir and heat to 145±3°C, dissolve, then add 17.68g of 1-(1-(4- (Benzyloxy)-phenyl)-2-(dimethylamino)-ethyl)-cyclohexanol; the mixture was reacted at 145°C under the protection of nitrogen, while continuously collecting the separated water, stirring and reacting for 12 hours, and then After cooling to room temperature, 290 ml of ethyl acetate and 200 ml of water were added to the mixture. The mixture was cooled (below 0° C.) and left overnight, and a solid precipitated out, which was filtered by suction and dried to obtain 10.65 g of O-desmethylvenlafaxine.
[0030] The yield is about 81.0%, the HPLC purity is 99.02%, MS: 264.22 (M+1). The detection result of product is shown in Figure 1, wherein Figure 1a is the HPLC spectrum, Figure 1b is the MS spectrum, Figure 1c for 1 H-NMR spectrum (English in the figure h...
Embodiment 2
[0033]Under the protection of nitrogen, add 23.4g of anhydrous sodium sulfide and 50ml of N-methylpyrrolidone to the three-necked flask successively, stir and heat to 145±3°C, dissolve, then add 17.68g of 1-(1-(4-(benzyloxy) -Phenyl)-2-(dimethylamino)-ethyl)-cyclohexanol; the mixture was reacted at 145°C under nitrogen protection, stirred for 12 hours, then allowed to cool to room temperature, the mixture was added with 290ml ethyl acetate, 200ml water. The mixture was cooled (below 0° C.) and left overnight, and a solid precipitated out, which was filtered by suction and dried to obtain 10.97 g of O-desmethylvenlafaxine.
[0034] The yield is about 83.5%, the HPLC purity is 99.42%, MS: 264.22 (M+1).
Embodiment 3
[0036] Under the protection of nitrogen, add 16.82g sodium hydrosulfide and 50ml N-methylpyrrolidone to the three-necked flask successively, stir and heat to 145±3°C, dissolve, then add 17.68g 1-(1-(4-(benzyloxy)- Phenyl)-2-(dimethylamino)-ethyl)-cyclohexanol; the mixture was reacted at 145°C under nitrogen protection, stirred and reacted for 12 hours, then allowed to cool to room temperature, and the mixture was added with 290ml ethyl acetate and 200ml water . The mixture was cooled (below 0° C.) and left overnight, and a solid precipitated out, which was filtered by suction and dried to obtain 10.21 g of O-desmethylvenlafaxine.
[0037] The yield is about 77.8%, the HPLC purity is 98.12%, MS: 264.22 (M+1).
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