Evaluation of a commercial packed bed flowhydrogenator for reaction screening, optimization, and synthesis

Beilstein Journal of Organic Chemistry

Volumn 7, Issue , 2011, Pages 1141-1149

  Bryan, Marian C ^a   Wernick, David ^a   Hein, Christopher D ^a   Petersen, James V ^a   Eschelbach, John W ^a   Doherty, Elizabeth M ^a  

^a AMGEN INC   (United States)

Author keywords

Catalyst leaching; CatCart ; H Cube ; Packed bed flow hydrogenation

Indexed keywords

EID: 80052043614     PISSN: 18605397     EISSN: 18605397     Source Type: Journal    
DOI: 10.3762/bjoc.7.132     Document Type: Article

References (25)

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21. The AutoH3 system was washed by replacing the solvent reservoirs (at both the Gilson and the Knauer pump) with wash solvent, then injecting 1.9 mL wash solvent through each CatCart Changer™ port position (quartz CatCart® cartridges), sequentially, and collecting 10 mL of wash solvent per injection.
22. The SAH3 system was washed by replacing the solvent reservoir with wash solvent and installing a 30 mm quartz CatCart® in the holder. Wash solvent was pumped at a rate of 1.0 mL/min for 10-40 min per solvent, with the system set to the full H2 mode at 30 °C.
23. Back-flushing was performed by plumbing directly from the Knauer pump to the outlet pressure sensor, with flow direction reversed, and disconnecting the remaining plumbing. The sensor was flushed with MeOH (15 mL, 3 mL/min), 10% HNO3 (100 mL, 2 mL/min), water (100 mL, 2 mL/min), and DMF (10 mL by syringe).
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