Diisopentyl ether → diisoamyl ether DEAC

Participants

Reaction Steps

n-Hexane (6 l), diethylaluminum monochloride (DEAC) (5.0 mols) and diisoamyl ether (12.0 mols) were mixed at 25° C. for 5 minutes, followed by reacting these at the same temperature for 5 minutes to obtain a reaction fluid (I) (the molar ratio of diisoamyl ether/DEAC:2.4). TiCl4 (40 mols) was introduced into a reactor equipped with a stirrer and purged with nitrogen and heated to 35° C., followed by dropwise adding thereto the total quantity of the above reaction fluid (I) over 180 minutes, thereafter keeping the mixture at the same temperature for 30 minutes, raising the temperature up to 75° C., further reacting it for one hour, cooling down to room temperature, removing the supernatant, and four times repeating a procedure of adding n-hexane (30 l) and removing by decantation to obtain a solid product (II) (1.9 Kg).

Provenance & Evidence