Diisopentyl ether → diisoamyl ether DEAC

n-Hexane (60 ml), diethylaluminum monochloride (DEAC) (0.05 mol) and diisoamyl ether (0.12 mol) were mixed together at 25° C. for one minute and then reacted at the same temperature for 5 minutes to obtain a reaction product liquid (the molar ratio of diisoamyl ether/DEAC:2.4). TiCl4 (0.4 mol) was introduced into a reactor purged with nitrogen and heated to 35° C. The total amount of the above reaction product liquid was dropwise added thereto over 3 hours and the mixture was kept at the same temperature for 30 minutes, followed by elevating the temperature up to 75° C., reacting it further for one hour, cooling down to room temperature, removing the supernatant liquid, and 4 times repeating a procedure of adding 400 ml of n-hexane and removing the supernatant liquid by decantation to obtain 19 g of a solid product. The total amount of this solid product was suspended in 300 ml of n-hexane, and to the resulting suspension were added diisoamyl ether (16 g) and TiCl4 (35 g) at room temperature (20° C.) over about one minute, followed by reaction at 65° C. for one hour. After completion of the reaction, the liquid was cooled down to room temperature (20° C.), followed by removing the supernatant liquid by decantation, 5 times repeating a procedure of adding 400 ml of n-hexane, stirring for 10 minutes, still standing and removing the supernatant liquid, and drying the resulting liquid under reduced pressure (1 mmHg) at 20° C. for 30 minutes to obtain a solid product (IV) (this solid product obtained in this Example will hereinafter be referred to as solid product (IV-1)). The TiCl3 content in 1 g of this solid product (IV-1) was 85% by weight.

1. customreacted at the same temperature for 5 minutes

ORD record

ord-f11318d2783347689f0cf5aa4c270d04

Source dataset

uspto-grants-1983_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04420593