Ferrocene-containing monomers and polymers and process for preparing same

• US 3,350,369 A
• Filed: 06/02/1964
• Issued: 10/31/1967
• Est. Priority Date: 06/02/1964
• Status: Expired due to Term

• Current Assignee: Gust Cottis Steve, Harold Rosenberg
• Original Assignee: Gust Cottis Steve, Harold Rosenberg
• Inventors: Rosenberg, Harold, GUST COTTIS STEVE
• Application Number:
  US04/372,128
• Time in Patent Office: 1,246 Days
• US Class Current: 526/238
• CPC Class Codes: C07F 17/02 of metals of Groups 8, 9 or 10 of the Periodic System
• CPC Class Codes: C08G 61/00 Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule C08G2/00 - C08G16/00 take precedence

Claims

3. THE PROCESS FOR MAKING POLY(1,2-OR 1,3-CYCLOPENTYLENE-1,2-OR 1,3-FERROCENYLENE) BY DISSOLVEING 0.2 MOLE OF FERROCENE IN 700 MILLILITERS OF ANHYDROUS METHYLENE CHLORIDE AT A TEMPERATURE BETWEEN 0*C. AND 5*C.;

ADDING TO THE SOLUTION 0.15 MOLE OF ANHYDROUS GRANULAR ALUMINUM CHLORIDE WITH STIRRING FOR 5 HOURS;

STIRRING THE SOLUTION AT ROOM TEMPERATURE FOR 16 HOURS;

POURING THE SOLUTION SLOWLY WITH STIRRING INTO 1000 MILLILITERS OF WATER;

ADDING TO THE SOLUTION 45 GRAMS OF SODIUM SULFITE WITH CONTINUOUS STIRRING;

FILTERING THE SOLUTION;

SEPARATING THE METHYLENE CHLORIDE LAYER;

REMOVING THE SOLVENT BY EVAPORATION TO ISOLATE THE RESIDUE;

ADDING 100 MILLILITERS OF HOT CYCLOHEXANE TO THE RESIDUE;

COOLING THE MIXTURE;

FILTERING THE MIXTURE;

EVAPORATING THE FILTRATE TO DRYNESS AS A DARKBROWN RESIDUE;

ADDING 200 MILLILITERS OF BOILING DIETHYL ETHER TO THE RESIDUE;

FILTERING THE ETHER AND RESIDUE MIXTURE WITH STIRRING INTO 1000 MILLILITERS OF METHANOL;

SEPARATING BY FILTRATION FROM THE METHANOL-ETHER SOLUTION A YELLOW SOLID THAT PRECIPITATES ON STANDING;

CONCENTRATING THE METHANOL-ETHER FILTRATE TO A TOTAL VOLUME OF 300 MILLILITERS;

CAUSING THE SOLUTION TO STAND AT 0*C. FOR 16 HOURS TO PERMIT A RESINOUS MATERIAL TO PRECIPITATE FROM THE SOLUTION;

DECANTING OFF THE SUPERMATENT LIQUID FROM THE RESINOUS MATERIAL;

DISSOLVING THE RESINUOUS MATERIAL IN 150 MILLILITERS OF PETROLEUM ETHER;

CHROMATOGRAPHING THE SOLUTION OF A COLUMN CONTAINING ACTIVATED NEUTRAL ALUMINA TO FORM SEVERAL BANDS ON THE COLUMN FROM THE PETROLEUM ETHER SOLUTION;

ELUTCHING THE LOWEST BAND WITH PETROLEUM ETHER;

THEREAFTER ELUTING THE SECOND BAND WITH CYCLOHEXANE;

THEN ELUTING THE MAIN BAND WITH DIETHYL ETHER;

AND EVAPORATING THE SOLVENT FROM THE MAIN BAND TO ISOLATE THE PRODUCT HAVING COMPOSITION (C15H16FE)N AS DETERMINED BY ELEMENTAL CHEMICAL ANALYSIS.