Ferrocene-containing monomers and polymers and process for preparing same
First Claim
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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.
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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.
- ADDING TO THE SOLUTION 0.15 MOLE OF ANHYDROUS GRANULAR ALUMINUM CHLORIDE WITH STIRRING FOR 5 HOURS;
Specification