Derivatives and Process for Their Preparation

Patent Cyclopentadienyl Derivatives and Process for Their Preparation 

Utility Co-components in Zirconium or Titanium Catalysts in a-Olefin 

A solution of cycloheptanone (0.5 mol), diethyl succinate (0.63 mol) dissolved in 500 ml DMF and potassium t-butoxide (0.67 mol) were mixed together while maintaining the temperature between 20 and 30°C. After 2 hours the mixture was poured into 2L of water, HCl added to obtain a pH = 2-3, and the product extracted with diether ether and isolated in 99% yield. 

The product from Step 1 was added to a mixture of 400 g 85% H3PO4 and 650 g P2O5 then heated to 90-95 °C 4 hours. The mixture was hydrolyzed with water, extracted with diethyl ether, and a 65% yield of crude product isolated. The material was purified by dissolving in 100 ml HO Ac, 100 ml water and 10 ml concentrated HCl and refluxing overnight. After neutralization, drying, and solvent removal the product was isolated in 64% yield. 

The product from Step 2 (16 g) was dissolved in 200 ml diethyl ether, LiAlH4 (3 g) mixed in 300 ml diethyl ether added, and the reaction stirred between 5 and 10°C. The mixture was hydrolyzed, extracted with ether, purified by chromatography on silica gel using petroleum ether and the product isolated in 98% yield. 

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