Pressure Chemistry Services

Peakdale’s state of the art and dedicated pressure laboratories are extremely well equipped to offer our customers a diverse range of chemistry capabilities. Our vast experience in low to high pressure (stp to 200 bar/3000 PSI) chemical transformations has been carefully built over many years of safe operation.

 

Pressure chemistry carried out at Peakdale includes:

  • Amination

  • Kolbe-Schmitt

  • Hydrolysis

  • Hydrazine Formation

  • Carbonylation

  • Hydroformylation

  • Chlorination   

  • Displacement Reactions

                             

Pressure chemistry plays an increasingly important role in modern organic synthesis, particularly in the production of APIs, intermediates and products for the fine chemical industry. At Peakdale, we now execute in excess of 500 synthetic chemistry projects annually with an extremely high level of success. We can apply our expertise to develop safe, efficient and cost effective routes for your pressure chemistry needs.

 

 High Pressure Reaction Equipment

Peakdale has a large array of Parr and Buchi apparatus - reactors from 5 ml to 20 L, stainless to Hastelloy - delivering material from reaction screens (mg) to scale up (kg). In the near future, we also expect to offer GMP quality pressure chemistry.

 

CASE STUDY

A client requested a synthesis of (150g) of the substituted pyridine-2-carboxamide derivative (2). After the synthesis of pyridine (1), Palladium catalysed carbonylation was attempted under 1 atmosphere (atm) of carbon monoxide. The reaction did not proceed to completion, even with the additional catalyst and reaction time. Formation of the debrominated impurity (3) was observed (Table 1).

 

The reaction was then optimized under high pressure conditions using a 300 ml autoclave. The reaction was performed at 10, 20 and 30 atm’s of carbon monoxide and then analysed by LCMS. At lower pressure 10 and 20 atm the formation of impurity (3) was still observed. However, gratifyingly, only the desired product (2) was observed at 30 atm.


Safe in the knowledge of the optimal reaction conditions, the synthesis was scaled up using the 2 L autoclave. The reaction completed as expected and the crude product was purified by crystallization.  

Compound (2) was then returned to the 2 L autoclave with methanolic ammonia, which upon heating to 100°C in the sealed system gave rise to the final target (4). Compound (4) was isolated by pouring the reaction mixture on to water and precipitation gave 167g of the customer’s desired compound which was delivered on time and in full.

 

For more information, please contact us at enquiries@peakdale.co.uk