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ChemicalBook CAS DataBase List 3,5-Dimethylpiperidine
35794-11-7

3,5-Dimethylpiperidine synthesis

2synthesis methods

3,5-Dimethylpiperidine can be prepared by catalytic hydrogenation of 3,5-dimethylpyridine (3, 5-dimethylpyridine, DPY). The reaction process was carried out in a droplet bed reactor (TBR) for Ru/C-catalyzed DPY, which has the advantages of high catalyt

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Yield:35794-11-7 99.5 %Chromat.

Reaction Conditions:

with 5% active carbon-supported ruthenium;hydrogen;acetic acid in water at 90; under 22502.3 Torr; for 8 h;Autoclave;Reagent/catalyst;Time;

Steps:

4.1-4.4 Example 4:
The method for screening a 3,5-lutidine derivative catalytic hydrogenation reaction by means of ORP data in the present example is as follows: 1. Dissolve 2.14g of 3,5-methylpyridine in 15-20mL water, 30%-50% glacial acetic acid, 5-15% hydrochloric acid aqueous solution (V/V), 5-10% phosphoric acid aqueous solution (V/V) a possible medium system for obtaining a substrate for catalytic hydrogenation reaction;2. The ORP of each of the above systems is separately tested; based on the measurement results, the catalytic hydrogenation reaction of 3,5-methylpyridine may have a higher oxidation performance of 40% acetic acid and 10% hydrochloric acid aqueous solution;3. 21.4g of 3,5-lutidine is dissolved in about 200mL of acetic acid or hydrochloric acid aqueous solution, catalyzed by 5% Ru/C, and the added amount is 5%, 10% substrate mass; the hydrogen pressure in the reaction kettle is controlled at 3 -4MPa, temperature 80-100 ° C, when the hydrogen pressure is no longer reduced, sample and monitor the conversion of 3,5-lutidine, filter the reaction solution in different reaction stages, measure ORP and piperidine, combine raw material conversion, The results of piperidine content and initial ORP change analysis 3,5-dimethylpyridine hydrogenation reaction suitable reaction medium ORP range of 370-410mV, catalytic addition amount of 10%, reaction pressure of 3.0MPa and temperature of 90 ° C; 4. Fix 5% Ru/C catalytic addition amount 10%, reaction pressure 3.0MPa and temperature 90 °C, adjust the concentration of 3,5-lutidine system 1.5mol/L and acidity of acid water reaction medium to make ORP at 375 -385, near 395-405mV, and then catalytic hydrogenation reaction again, the reaction was sampled at about 6h, 8h, GC area normalization method to detect 3,5-lutidine and 3,5-dimethyl under different ORP schemes The percentage of piperidine area is:Considering the conversion rate of 3,5-methylpyridine and the content of 3,5-dimethylpiperidine product, it is preferred that the preparation process of 3,5-lutidine is: 1.5 mol/L substrate concentration, 10% HCl (ORP 380 mV) or 45% aqueous acetic acid solution (ORP 380 mV) is the reaction medium, 5% Ru/C catalytic addition amount 10%, temperature 90 ° C, hydrogen pressure 3.0 MPa, and the reaction is completed under the conditions of about 8 h.

References:

Anhui Dexinjia Bio-pharmaceutical Co., Ltd.;Xu Kun;Hui Ailing;Zhang Wencheng;Wu Zeyu;Chen Tianyun;Wang Zhiyong CN109678789, 2019, A Location in patent:Paragraph 0060-0068

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