Two preparation methods of tris(hydroxymethylaminomethane) are big PK

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Tris in English and 2-Hydroxymethyl-2-nitro-1,3-propanediol in English. It is an important biochemical, chemical and pharmaceutical intermediate. Tris is the most common buffer component and titration standard in biochemical and molecular biology experiments. As a drug, it can effectively treat acidosis in patients with acute lung injury and induce phospholipid bilayer membranes to form monolayer membranes with corrugated structures. At the same time, it is also widely used as a solvent for nucleic acids and proteins, as well as many other important uses.

Here are two methods for the preparation and synthesis of tris.

1) Direct hydrogenation method

Put the condensation reaction solution into a 2.0 L autoclave, add 650 mol methanol, 10 mol dichloromethane, and 12 g Raney nickel. After the autoclave has passed the leak test, switch it with nitrogen and hydrogen 4 to 5 times, start the stirrer, and adjust the speed. Slowly increase the temperature, then add hydrogen, the reaction temperature rises to the specified temperature, and react for 2.5 h at the specified temperature and pressure. After the reaction is over, the filtrate is poured into a beaker, cooled to -5°C with brine, and the white crystals are separated out. After filtration, the filtrate was concentrated under reduced pressure, and then cooled to crystallize and suction filtered, treated in the same way for 3 times, and the product was dried in vacuum.

2) Two-step method

Weigh 120 g of tris (hydroxymethyl) nitromethane (THNM), 500 g of methanol, 15 g of dichloromethane, and 12 g of Raney nickel (wet product), and add them to the autoclave in sequence. After the autoclave passed the leak test, replace it with nitrogen and hydrogen 4 to 5 times, start the stirrer, and adjust the speed. Slowly increase the temperature, then add hydrogen, the reaction temperature rises to 50-55°C, the pressure is 2.0-2.5MPa, the reaction is at this temperature for 2.5h, after the reaction, the catalyst is filtered off, the reaction liquid is cooled and crystallized, and the product is vacuum dried.

Direct hydrogenation test results

The direct hydrogenation method to produce trishydroxymethylaminomethane was optimized under different conditions according to the above experimental method. The results are listed in Table 1.

Two-step production of tris(hydroxymethyl)aminomethane

After nitromethane is condensed with aqueous formaldehyde solution, the average yield of direct hydrogenation to produce trishydroxymethylaminomethane is low (below 50%) and does not meet the conditions for large-scale industrial production. Therefore, the condensation method of aqueous formaldehyde solution is used in the production to produce three Hydroxymethyl nitromethane is a two-step production process for separating trimethylol nitromethane and then hydrogenating and reducing it to produce trimethylolaminomethane. It can be seen from Table 2 that the effect of different reaction conditions on the yield.

The direct method and the two-step method to produce tris, the process is stable, but the yield of the tris produced by the direct hydrogenation method is lower than that of the two-step method. The most important thing is that the production cost of the direct hydrogenation method is higher than the cost of the two-step method, so it is recommended to use the two-step method to produce tris.

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