Methods and apparatus for liquid phase separation

Liquid purification or separation – Processes – Liquid/liquid solvent or colloidal extraction or diffusing...

Reexamination Certificate

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C210S644000, C210S321600, C210S321840, C422S105000, C436S177000

Reexamination Certificate

active

06183645

ABSTRACT:

TECHNICAL FIELD
The present invention relates to processes and devices for phase separation of materials, particularly for use in multiple, simultaneous synthesis, purification and isolation of compounds.
BACKGROUND ART
Various apparatus and methods are known for the multiple, simultaneous synthesis of compounds, including, but not limited to, organic compounds. Some of the preferred methods and apparatus are shown, for example, in U.S. Pat. No. 5,324,483 entitled “Apparatus for Multiple Simultaneous Synthesis,” which is assigned to the same assignee as the present invention. In accordance with that patent, a plurality of compounds are simultaneously synthesized in an array format which is compatible with standard techniques of organic synthesis. The sample handling is carried out using automated systems for speed, accuracy and precision.
The method and apparatus disclosed in the '483 patent can be used for either solid (resin) support or solution based synthesis techniques. The primary steps necessary to perform the synthesis are the development of a synthetic route that will be feasible with the solid or solution techniques utilized, the verification of the synthesis using representative examples, and the execution of the multiple, simultaneous synthesis within an array format to generate the plurality of compounds.
The '483 patent increases the flexibility and diversity of structures that can be produced by parallel, solid phase or solution-based chemical synthesis. Where solution-based chemistry is involved, typically two-phase liquid/liquid extraction protocols are utilized. These techniques are not as easily amenable to automation as techniques using solid or resin-support techniques.
SUMMARY OF THE INVENTION
It is an object of the present invention to provide an improved apparatus and method for phase separation. It is also an object of the present invention to provide a phase separation apparatus and method which is useful for multiple, simultaneous synthesis, purification and isolation.
It is a further object of the present invention to provide a two-phase separation apparatus and method which is more amenable to automation and thus which will facilitate a more efficient and faster simultaneous, multiple synthesis, purification and isolation of compounds.
It is still another object of the present invention to provide a phase separation device which is less expensive and easier to manufacture than known separation devices and which also can be provided a disposable form.
These and other objects are met by the present invention which provides an improved apparatus and method for phase separation of different materials. In accordance with the present invention, a hydrophobic paper filter disk is retained on top of or between porous filter devices in the lower end of a phase extraction cartridge. The cartridge has an open end in which the solution or slurry of materials is introduced, often with a solvent, and a lower end which has an outlet for draining and collection of the separated non-hydrophobic materials. Preferably, the separated material is also passed through a drying cartridge attached to or positioned immediately adjacent the exit of the cartridge.
When used for reaction workup and quenching, the crude reaction mixture is introduced into the cartridge containing an aqueous reaction quenching or workup solution, such as water or saturated ammonium chloride. The introduction of additional solvents or reagents to facilitate a two-phase medium is preferred when using aqueous miscible reaction solvents or mixtures. The heavier materials are separated by passing through the frits and hydrophobic paper filter disk, and the separated material is then dried by passing it through the drying cartridge.
These and other features and benefits of the present invention will become apparent when the following description is viewed in accordance with the attached drawings and appended claims.


REFERENCES:
patent: 3295686 (1967-03-01), Krueger
patent: 4221670 (1980-09-01), Ziemek
patent: 5096585 (1992-03-01), Nguyen
patent: 5133934 (1992-07-01), Denton
patent: 5186830 (1993-02-01), Rait
patent: 5240680 (1993-08-01), Zuckermann
patent: 5324483 (1994-06-01), Cody
patent: 5464541 (1995-11-01), Aysta
patent: 5529694 (1996-06-01), Strickler
patent: 5874004 (1999-02-01), DeWitt

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