Method for synthesizing N-(3-methoxy propyl)-4-amino-piperidine
A technology of methoxypropyl and aminopiperidine is applied in the synthesis field of N-(3-methoxypropyl)-4-aminopiperidine, which can solve the problems of difficult industrialization, difficult filtration and the like, and achieves the Easy to handle, easy to handle and store, inexpensive effect
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example 1
[0060]
[0061] At room temperature, in a 250ml three-neck flask, add 17.1g N-(3-methoxypropyl)piperidone, 10.7g benzylamine, 100ml methanol, stir and dissolve, then add 21.2g triacetyl borohydrogenate After adding sodium, after stirring at room temperature for 4 hours, the conversion was complete as monitored by TLC. Add 100ml of dilute hydrochloric acid with a concentration of 0.1mol / L to quench, evaporate the solvent under reduced pressure, add 100ml of water and 100ml of ethyl acetate, stir and separate, keep the organic layer, extract the aqueous layer twice with ethyl acetate, and combine the organic Mutually. The organic phase was washed twice with water, dried over anhydrous magnesium sulfate for 4 hours and concentrated to obtain 21.6 g of oil, with a molar yield of 82.3%.
[0062] Example 2-5 is to screen the substituted benzylamine of this step reaction, and charge ratio, experimental operation are all identical with example 1,
[0063] The results are shown in...
example 4
[0066] The concrete operation of example 4 is as follows:
[0067] At room temperature, in a 250ml three-necked flask, add 17.1g of N-(3-methoxypropyl)piperidone, 13.7g of p-methoxybenzylamine, and 100ml of methanol. After stirring and dissolving, add 21.2g of After sodium triacetylborohydride was stirred at room temperature for 4 hours, the conversion was complete as monitored by TLC. Add 100ml of dilute hydrochloric acid with a concentration of 0.1mol / L to quench, evaporate the solvent under reduced pressure, add 100ml of water and 100ml of ethyl acetate, stir and separate, keep the organic layer, extract the aqueous layer twice with ethyl acetate, and combine The organic phase. The organic phase was washed twice with water, dried over anhydrous magnesium sulfate for 4 hours and concentrated to obtain 23.2 g of an oily substance with a molar yield of 88.6%.
[0068] Example 6-7 is to screen the solvent of this step reaction, and charging ratio and operation are identical w...
example 11
[0073]
[0074] At room temperature, in a 250ml three-neck flask, add 13.1g of intermediate C-1 and 100ml of methanol, stir until dissolved, add 3g of 10% palladium carbon, and pass in hydrogen gas under normal pressure, and react for more than 12 hours. After the conversion of raw materials is monitored by TLC , filter out the palladium carbon, add dropwise 100ml concentration of 2mol / L HCl ethanol solution to the filtrate, after a large amount of solids appear, continue to stir for more than 4 hours, filter to obtain a white solid, weigh 11.8g after drying, and the molar yield is 96.3%.
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