Method for purifying venlafaxine intermediate

The invention relates to a method for purifying a venlafaxine intermediate. The method is characterized by comprising the steps that a 1-[2-amino-1-(p-methoxyphenyl)ethyl]cyclohexanol crude product isadded into a solvent, then acid is added, the mixture is cooled to 10-20 DEG C, solid is slowly sepa...

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Bibliographische Detailangaben
Hauptverfasser: SUN FUQIANG, LI DAJUAN, LI HONGGONG
Format: Patent
Sprache:chi ; eng
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Beschreibung
Zusammenfassung:The invention relates to a method for purifying a venlafaxine intermediate. The method is characterized by comprising the steps that a 1-[2-amino-1-(p-methoxyphenyl)ethyl]cyclohexanol crude product isadded into a solvent, then acid is added, the mixture is cooled to 10-20 DEG C, solid is slowly separated out, and the solid obtained through filtering is washed for 1-3 times with a solvent at the temperature of -5-10 DEG C; then the washed solid is added into water to be dissolved, and then an alkali solution is added to adjust the PH value to be larger than 9; then an organic layer is extracted with ethyl acetate, and the organic layer is concentrated under reduced pressure to be dry, and high-purity pure 1-[2-amino-1-(p-methoxyphenyl)ethyl]cyclohexanol is obtained. The method has the advantage of purifying the venlafaxine intermediate at a high yield. 本发明涉及种文拉法辛中间体的纯化方法,其特征为将1-[2-氨基-1-(对甲氧苯基)乙基]环己醇粗品加入到溶剂中,再加入酸后冷却至10~20℃,缓慢析出固体,过滤得到的固体,将固体用的-5~10℃的溶剂洗涤1~3次;再将洗涤后的固体加入到水中溶解,然后再加入碱溶液调节PH值大于9,然后用乙酸乙酯萃取有机层,将有机层减压浓