Optimization of a hydrogenation process using real-time mid-IR, heat flow and gas uptake measurements

Organic Process Research and Development

Volumn 14, Issue 6, 2010, Pages 1512-1517

  Littler, Benjamin J ^a   Looker, Adam R ^a   Blythe, Todd A ^a  

^a VERTEX PHARMACEUTICALS   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

GAS UPTAKE; HEAT FLOWS; HYDROGENATION PROCESS; REACTION CONDITIONS;

AROMATIC COMPOUNDS; HEAT TRANSFER; HYDROGENATION; OPTIMIZATION; PILOT PLANTS; REACTION RATES;

REACTION INTERMEDIATES;

EID: 78649671995     PISSN: 10836160     EISSN: 1520586X     Source Type: Journal    
DOI: 10.1021/op100169j     Document Type: Article

References (10)

1. http://www.fda.gov/Cder/OPS/PAT.htm.
2. http://www.ich.org.
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4. Baumeister, P.; Blaser, H.-U.; Studer, M. Catal. Lett. 1997, 49, 219
5. http://en.wikipedia.org/wiki/Infrared-spectroscopy.
6. Minnich, C. B.; Buskens, P.; Steffens, H. C.; Bäuerlein, P. S.; Butvina, L. N.; Küpper, L.; Leitner, W.; Liauw, M. A.; Greiner, L. Org. Process Res. Dev. 2007, 11, 94
7. Mettler Toledo AutoChem, Inc., 7075 Samuel Morse Drive, Columbia, MD 21046, United States.
8. An experiment was performed where samples were removed approximately every 15 min for HPLC analysis. This confirmed that that the changes in the mid-IR bands measured from peak height to baseline correlated to the chemical transformations under investigation.
9. HPLC analysis of the final product mixture showed much cleaner conversion of 1 to 2 compared to using the Pd/C catalyst.
10. Platinum: $1220.90/Troy oz; palladium $238.50/Troy oz NYMEX Close April 15, 2009.