Liquid purification or separation – With means to add treating material – Chromatography
Reexamination Certificate
2002-05-01
2003-11-18
Therkorn, Ernest G. (Department: 1723)
Liquid purification or separation
With means to add treating material
Chromatography
C210S243000, C210S656000, C210S748080, C422S070000
Reexamination Certificate
active
06649051
ABSTRACT:
TECHNICAL FIELD
The invention relates to processing of chemicals in flow-through devices with porous media.
U.S. Pat. No. 6,139,733, which is hereby incorporated by reference, describes a sample module made of a flow-through device that contains porous media and describes adding a chemical sample to the module prior to connecting the module to (or inserting the module into) a chromatography column. The sample can be added to the module in a dissolution solvent that can be removed by vacuum or heat prior to connection to the chromatography column.
SUMMARY
In one aspect, the invention features, in general, processing a chemical sample by introducing a sample into a flow-through device containing a porous solid media therein, and thereafter subjecting the device to microwave energy.
In another aspect, the invention features, in general, introducing a chemical sample into a flow-through device containing a porous solid media therein and active components attached to the solid media, and thereafter subjecting the device to energy in order to accelerate reactions implemented by the active components, the reactions resulting in a reaction product created from the sample.
In another aspect, the invention features, in general, introducing reagents into a flow-through device containing a porous solid media therein and active components attached to the solid media, causing a synthesis reaction involving the reagents in the flow-through device and resulting in a reaction product, thereafter placing the flow-through device into an entrance region within a chromatography column, and thereafter carrying out chromatography on the reaction product.
In another aspect, the invention features, in general a chromatography sample module including a flow-through member having walls and having an inlet end and an outlet end; a solid porous media disposed within the flow-through member and including attached active components, the media being spaced from the inlet end so that the walls extend above the media and so that the flow-through member defines a receiving region adapted to receive a head piece; and a sample carried on the media.
In another aspect, the invention features, in general, a tubular member that is sized to fit entirely within the end of a chromatography column containing a separation media, the module having an inlet and an outlet, and solid porous media within the tubular member and spaced from the inlet, so that the tubular member defines a receiving region adapted to receive a head piece. The tubular member is sized to be sealed within the chromatography column with a sealing device used to seal the chromatography column. The solid porous media includes attached active components and carries a sample.
In another aspect, the invention features, in general a flow-through device having walls and having an inlet end and an outlet end; a solid porous media disposed within the flow-through device including attached active components, the media being spaced from the inlet end so that the walls extend above the media and so that the flow-through member defines a receiving region adapted to receive a head piece; and a sample carried on the media.
Particular embodiments of the invention may include one or more of the following features. In particular embodiments, the sample is introduced into the flow-through device in a solvent that is evaporated by microwave energy prior to carrying out chromatography. In some embodiments, the solid media includes active components attached thereto, and the microwave energy speeds up the reactions involving the active components. In some embodiments the sample includes reagents that undergo a chemical reaction to form a reaction product. The active components attached to the solid media can include scavengers to remove excess reagents. The scavengers can be electrophile scavengers, e.g., amino scavengers, TsNHNH
2
scavengers, or SH scavengers. The scavengers can be nucleophile scavengers, e.g., TsCl scavengers and NCO scavengers. The scavengers can be base scavengers, e.g., a quaternary amine scavenger. The scavengers can be acid scavengers, e.g., TsOH scavengers or COOH scavengers. The active components can be coupling agents, e.g., DCC coupling agents, HOBt coupling agents, or NHS coupling agents. The active components can be a catalyst, e.g., TsOH. The active components can be a catalyst remover, e.g., DEAM.
Embodiments of the invention may include one or more of the following advantages. The use of microwave energy to evaporate solvent in a flow-through device in which a sample carried in a solvent has been absorbed onto solid media in the flow through device greatly speeds up and simplifies the evaporation process. Attaching active components to the solid media in a flow-through device that can be used to introduce a sample into a chromatography column, permits the same device to be used as a reaction chamber and sample introduction device, simplifying and speeding up synthesis and purification. Subjecting the device with solid media and attached active components to microwave or other energy speeds up the synthesis or other reactions therein.
Other features and advantages of the invention will be apparent from the following detailed description and from the claims.
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patent: 6530260 (2003-03-01), Mustacich et al.
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Information from Personal Chemistry website www.personalchemistry.com undated pp. 1-6.
Information from CEM website www.CEM.com undated pp. 1-15.
Information from Milestone Inc. Website www.milestonesci.com/SYN%Features.htm pp. 1-14 Aug. 30, 2002.
Hammond Kelvin
Horsman Jeffrey A.
Jamalabadi Shahnaz Ghassemi
Mneimne Omar
Rahn Peter C.
Biotage Inc.
Fish & Richardson P.C.
Therkorn Ernest G.
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