Synthesis of N-silylated cyclopentaphenanthrene compounds

A method which comprises:

• (i) reacting 2,3-dehydro-1-oxycyclopentaphenanthrene with tosylhydrazide having the formula ##STR11## in a non-interfering solvent wherein a tosylhydrazone compound having the formula:
• ##STR12## is produced;
• (ii) reacting the tosylhydrazone produced in step (i) with LiN(R).sub.2 wherein R is a one to six carbon atom alkyl group, in a non-interfering medium to produce .sup.1 H cyclopentaphenanthrene having the formula:
• ##STR13## (iii) reacting the .sup.1 H cyclopentaphenanthrene product of step (ii) with butyl lithium and CH.sub.3 SO.sub.3 Si(CH.sub.3).sub.2 (t-butyl) wherein an N-silylated compound having the formula:
• ##STR14## wherein R is n alkyl group is produced;
• (iv) reacting said n-silylated compound produced in step (iii) with Ti(NMe.sub.2).sub.4 and (Me).sub.3 SiCl wherein a titanocene compound having the formula:
• ##STR15## is produced.

A method which comprises

• (i) reacting cyclopentaphenanthrene with butyl lithium in a mixed toluene and ether solvent
• wherein a first reaction mixture containing lithiated cyclopentaphenanthrene in said solvent mixture is produced;
• and
• (ii) reacting CH.sub.3 SO.sub.3 Si(CH.sub.3).sub.2 NHR with said lithiated cyclopentaphenanthrene contained in step (i) first reaction mixture
• wherein a second reaction mixture is produced and
• wherein said second reaction mixture contains the compound ##STR16## wherein R is an alkyl group.