Titanium Tetrachloride → HCID 131731263, compound

Participants

Reaction Steps

Solution of 4.00 g (15.15 mmol) of 2-tert-butyl-4,5-di-tert-pentyl-imidazole in 10 ml of toluene was added to 22.7 ml of 1 M TiCl4 in toluene (22.7 mmol) at RT during ˜5 minutes. The solution turned dark and formation of yellow precipitate was observed. The slurry was agitated for 24 hours and large amount of solid was formed. The solid was filtered and washed with 20 ml of toluene. 4.45 g of yellow solid, which was likely a salt of 2-tert-butyl-4,5-di-tert-pentyl-imidazolium tri-mu-chlorido-bis[trichloridotitanium(IV)] (Ti2Cl9−). Toluene was distilled out from the filtrate under vacuum and residue was dried under vacuum at 95° C. to remove traces of unreacted TiCl4 and 2-tert-butyl-4,5-di-tert-pentyl-imidazole (light yellow liquid). The residual material was transferred into 25 ml flask and sublimed under 0.2 torr at 80-100° C. to obtain 1.1 g of deep red solid (17% yield based on 2-tert-butyl-4,5-di-tert-pentyl-imidazole).

Provenance & Evidence