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Zone Refining of Diethylaminostyrlpyrazoline (DEASP) and Methoxy DEASP

IP.com Disclosure Number: IPCOM000084878D
Original Publication Date: 1976-Jan-01
Included in the Prior Art Database: 2005-Mar-02
Document File: 1 page(s) / 11K

Publishing Venue

IBM

Related People

Duran, J: AUTHOR

Abstract

Diethylaminostyrlpyrazoline (DEASP) and methoxy-DEASP cannot be zone refined alone, because alone they inherently supercool from a melt to form a glass.

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Zone Refining of Diethylaminostyrlpyrazoline (DEASP) and Methoxy DEASP

Diethylaminostyrlpyrazoline (DEASP) and methoxy-DEASP cannot be zone refined alone, because alone they inherently supercool from a melt to form a glass.

A 3:1 ratio, by weight, of biphenyl to each of the compounds permits their zone refining by preventing "glass" formation. The biphenyl in this ratio idealizes the viscosity and prevents separation of the mixture. Impurities are thus segregated due to the difference of solubility in the liquid and solid phase of the mixture.

Following multiple zone passes (50), the mixture is removed from the zone refining tube and placed into a vacuum sublimation apparatus. The biphenyl is then sublimed onto the cold finger. To ensure complete removal of traces of biphenyl, the bath temperature is raised to 145 degrees C (for DEASP) and 165 degrees C (for methoxy-DEASP). The sample is allowed to cool and subsequently the biphenyl collected is removed while the coolant still remains in the cold finger.

The compounds will be amorphous at this point but may be crystalized from n-hexane, ethyl acetate or other suitable solvent.

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