Dimethyltitanocene (CAS NO.: ), which is also known as , di-π-cyclopentadienyldimethyl-, could be produced through the following synthetic routes.

A 1-L, three-necked, round-bottomed flask, equipped for mechanical stirring, and outfitted with a 250-mL, pressure equalizing addition funnel, and a Claisen adapter bearing a thermometer and a nitrogen inlet/outlet vented through a mineral oil bubbler, is placed under a nitrogen atmosphere and charged with 41.5 g (0.167 mol) of titanocene dichloride, and 450 mL of dry . The slurry is efficiently stirred and chilled to an internal temperature of -5°C in a ice/methanol bath; then 126 mL of a 3 M solution (0.38 mol) of methylmagnesium chloride in tetrahydrofuran (THF) is added dropwise via the addition funnel over 1 hr, at a rate of addition adjusted to maintain an internal temperature below +8°C. The resulting orange slurry is mechanically stirred at an internal temperature of 0 to +5°C for 1 hr, or until the insoluble purple titanocene dichloride is no longer seen in the suspension. The addition funnel is removed and replaced by a rubber septum, and the reaction is assayed by 1H NMR.

While the reaction is aging at 0° to +5°C, a 2-L, three-necked, round-bottomed flask, equipped for mechanical stirring, and outfitted with a rubber septum, and a Claisen adapter bearing a thermometer and a nitrogen inlet/outlet vented through a mineral oil bubbler, is placed under a nitrogen atmosphere and charged with 117 mL of 6% aqueous ammonium chloride (7.0 g diluted to 117 mL). The solution is chilled to 1 to 2°C, with efficient mechanical stirring. When the formation of dimethyltitanocene is judged to be complete, the toluene /THF reaction mixture is quenched into the well-stirred aqueous ammonium chloride solution via a cannula over a period of 1 hr, maintaining an internal temperature of 0° to +5°C in both flasks. Toluene (30 mL) is used to rinse the reaction flask. The biphasic mixture is then poured into a 2-L separatory funnel, with another 30 mL of toluene rinse, and the aqueous phase is separated. The organic layer is washed sequentially with three portions of cold water (100 mL each) and brine (100 mL), then dried over anhydrous sodium sulfate (Na₂SO₄, 35 g). The organic layer is filtered and carefully concentrated under reduced pressure on a rotary evaporator at a bath temperature of no more than 35°C to a weight of 150 g. The resulting orange solution is assayed by 1H NMR to be 20 weight percent dimethyltitanocene (29.55 g, 85.0%). If the solution is to be stored for more than a week, the reagent should be diluted with 160 mL of dry THF, which has a stabilizing effect on the labile reagent. The solution is stored at 0° to 10°C under nitrogen in a rubber septum-sealed, round-bottomed flask. It proved effective in the conversion of a complex ester to an enol ether.