Method for purifying 2-[(4-chlorophenyl)(piperidin-4-yloxy)methyl]pyridine
A compound and organic solvent technology, applied in the field of high-purity products, can solve the problems of cumbersome industrial production, inability to continue, and time-consuming crystallization process, and achieve the effect of shortening purification time and high purity
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[0048] Example 1 Purification of Formula I (1)
[0049] Take 20 g of the crude product of formula I and dissolve it in dichloromethane, then add 5% hydrochloric acid to the solution to make the pH of the system 6.2, mix well and make it separate. The organic layer was discarded, and the pH of the aqueous layer was adjusted to 10.0 with sodium hydroxide, and then extracted with an appropriate amount of dichloromethane. The extract was dried, filtered, and concentrated to obtain 14.6 g of a red viscous liquid with a purity of 98.8%.
Example Embodiment
[0050] Example 2 Purification of Formula I (2)
[0051] Add 20ml of diethyl ether to 400ml of water, then adjust the pH of the system to 5.0 with glacial acetic acid, add 15g of the crude product of formula I to the above system to dissolve, mix evenly and make it separate. Separate the water layer, adjust the pH value to 8.5 with ammonia water, extract with an appropriate amount of chloroform, dry, filter, and concentrate the extract to obtain 15.8 g of a red viscous liquid with a purity of 99.1%.
Example Embodiment
[0052] Example 3 Purification of Formula I (3)
[0053] Take 15g of the crude product of formula I, dissolve it with toluene, add 160ml of water to the solution, then adjust the pH of the system to 8.0 with 10% p-toluenesulfonic acid, mix well and separate it into layers, discard the organic layer, and use hydrogen for the water layer. After adjusting the pH value of lithium oxide to 14.0, it was extracted with an appropriate amount of toluene, and the extract was dried, filtered, and concentrated to obtain 12.0 g of a red viscous liquid with a purity of 98.2%.
[0054] Example 4 Purification of Formula I (4)
[0055] Take 30g of the crude product of formula I and dissolve it with ethyl acetate, add 15ml of water to the solution, and then adjust the pH of the system to 7.4 with 10% sulfuric acid, mix well and allow it to separate into layers. The aqueous layer was separated and adjusted to pH 12.0 with potassium oxide, and then extracted with an appropriate amount of ethyl acetate. ...
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